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The commercial development of the shallow (2200 ft2 400 ft) Windalia sand reservoir at Barrow Island provided the opportunity to conduct an intensive drilling programme using equipment and techniques designed for optimum performance.During the initial exploratory and reservoir delineation phase, 12 specific Windalia test wells were drilled using drilling equipment with an optimum depth range of 6QOO ft - 8000 ft and a 9 5/8 in by 7 in. casing programme was employed. The average time from commencement of move-in to rig release exclusive of coring for five representative wells was 187 hr during this phase.Development drilling commenced December 1966 with one rig, with the second in operation January 1967.As of January 1 1968, 168 development wells had been completed. The two rigs employed are drive-in units equipped with a telescoping .gelf raising doubles mast.Optimum depth range with 4 1/2 in. drill pipe is 2500-4000 ft. Casing programme is 8 5/8 in. by 5 1/2 in. Efficient performance was achieved immediately. The average time from commencement of move-in to rig release for 15 wells drilled early in the development programme was 99 hr.By application of experience and further modification of techniques, performance was improved to an average time of 72 hr per well for 15 wells recently completed.The major drilling problem on Barrow Island is surface hole drilling due to the very hard surface limestone combined with complete loss of circulation at sea level.In this operation, significant improvements have been effected. During the exploratory phase drilling, 12 1/4 in hole to set 9 5/8 in. casing, average penetration rate was 23 ft/hr. At the commencement of the development programme penetration rate, drilling 10 5/8 in. hole to set 8 5/8 in. casing, was 28 ft/hr for the 15 early wells considered, improving to 55 ft/hr for the 15 recent wells considered.This programme is a team effort and much credit must be given to the enthusiastic co-operation of the two drilling contractors.The current field record is 2 days 4 hr with a 4 1/2 hr move including the drilling of mousehole and rathole.

Jan 1, 1968

By H. C. Rolseth, J. J. Calaman

6.4-1. Principles of Operation. The jet-piercing process is a patented thermal process which depends upon a characteristic of the rock which is termed spallability. In its simplest terms, spalling is considered as decrepitation resulting from differential expansion of rock crystals due to thermally induced stresses. The number of individual properties influencing the spalling characteristics of rock are so numerous and their interaction so complex that the only truly reliable way to ascertain the spallability of rocks under thermal shock conditions is to expose them to these conditions. However, laboratory and field work have determined the principal thermal, physical, and mechanical properties of rock which affect spallability (10, 18). The approximate relationship between spallability and these characteristics is as follows: [ ] where To is the critical temperature at which, it is believed, a rock becomes elastic or sufficiently plastic to prevent further spalling action. Thermal diffusivity takes into account the amount of heat used in saturating the medium itself during the migration of a heat front. The rate and degree of dimensional changes which influence the spalling tendency of the rock will depend upon the characteristic of the heat gradient in the rock. The greater the spalling tendency, the higher the piercing rate. Those properties most favorable to a high degree of spallability are: 1. Large linear thermal expansion at temperatures below 700°C. 2. High thermal diffusivity at temperatures below 400°C. 3. Equigranular interlocking structure with little or no fine-grained clay or mica alteration products. 4. No significant amounts of soft, low-melting, or elastic mineral or materials which yield after thermal decomposition.

Jan 1, 1968

By A. K. Jena, M. O. Bever

The thermodynamic behavior of dilute solutions of copper, silver, and gold in liquid tin is not explained by current solution theories.1-3 The relative partial gram-atomic enthalpies, or heats of solution, of silver, gold, and platinum in liquid lead at 623°K have been measured in the investigation reported here. Their interpretation requires a modification of the regular-solution theory although lead-rich solutions may be expected to be simpler than tin-rich solutions. The liquid metal solution calorimeter used has been described.4 At the start of a run the bath consisted of 621 g of reagent-grade lead. Several calibrating additions of lead were made during a run; a value of 3.48 kcal per g-atom5 was taken for H623°K - H273°K Two runs were made with each of the solutes silver, gold, and platinum. Annealed wire samples of 99.999+ pct purity were used. Four to six samples each weighing 0.5 to 1,0 g were added from 273°K to the bath at 623°K and the associated heat effects were measured. The samples dissolved in approximately 3 min. No serious experimental difficulties were encountered. The heat effects of the additions in a run plotted against the average atom fraction of solute before and after each addition314 were linear functions of the concentration in lead of silver, gold, and platinum, respectively. By subtracting the difference between the heat contents of a solute element at 623° and. 273°K5 from the measuredheat effects, the partial gram-atomic enthalpy relative to the solid solute was obtained. The relativ: partial gram-atomic enthalpy at infinite dilution and the concentration dependence of the partial gram-atomic enthalpies obtained from the plots of vs atomic fraction x are listed in Table I. The relative partial gram-atomic enthalpy at infinite dilution of silver in lead of 5.46 kcal per g-atom at 623°K compares with values at 723°K of 5.74' and 5.765 kcal per g-atom. These data yield a temperature coefficient of 3.0 cal per g-atom-OK. The partial gram-atomic enthalpy at infinite dilution of gold in lead at 623°K is 0.89 kcal per g-atom compared with 0.85 kcal per g-atoms (obtained by extrapolation) and 0.95 kcal per g-atom.5 By combining these values for 623°K with those for several other temperatures5" the temperature coefficient of was found to be 3.2 cal per g-atom-OK. No thermodynamic data are

Jan 1, 1968

By R. J. Schaefer, M. E. Glicksman

Direct, in situ observation of metallic alloys during solidification reveals that in some systems crystal multiplication occurs by means of a dendrite remelt-ing process, without the necessity of independent nu-cleation events. The solidification is observed on optically clean surfaces of supercooled molten alloys. In one system (Sn-3 wt pct Bi) , a fine-grained equi-axed structure is produced by the complete disintegration, via remelting, of transient initial dendrites. In contrast, several other metallic systems show little or no evidence of remelting activity. The behavior of these metallic systems is consistent with that expected on the basis of published observations of dendrite remelting in transparent organic alloy systems. It is concluded that dendrite remelting is an important crystal multiplication process in some metallic alloys, but is velatively unimportant in some other alloys. The detachment of dendrite branches from the primary stem by a remelting process has been observed by Jackson, Hunt, Uhlmann, and seward1 during the solidification of some transparent organic alloy systems. The branches released by this remelting process can drift free of the primary stem and serve as seeds for the formation of numerous independent crystals. This proliferation of new crystals does not require repeated independent nucleation events, but only modification of the initial solidification structure. The mechanism of dendrite remelting, as described by Jackson et a1.1 and by Tiller and O''Hara,2 is dependent on the transport of both heat and solute and is, therefore, expected to operate only in alloys, and not in pure substances. It was found in the transparent organic alloy systems that remelting occurred primarily in the constricted regions near the base of dendrite branches, where the branches had grown through the solute-rich liquid layer surrounding the primary dendrite stem. It was suggested that impure solid had formed in these constricted regions at a relatively low temperature and had later become unstable as further solidification of purer material raised the temperature. Jackson et al. proposed that the equiaxed zone of metal alloy castings originates from a similar remelting process, and they demonstrated the operation of this mechanism in "ingots" poured from saturated salt solutions. Although these substances were especially selected to show solidification behavior similar to that of metals,3 the remelting mechanism has, until now, been subject to the objection that its operation has not been directly observed in a metallic system. Considering the fact that thermal properties such as diffusivity may differ by as much as two or three orders of magnitude between metals and organic compounds, this objection was considered to be possibly serious. A method has now been developed by which it is possible to make direct optical observations of metals during solidification. This method has revealed transient solidification processes which would not be detected by metallographic examination of totally solidified specimens. In particular, a grain-refinement process in a metallic alloy has been observed to be a direct consequence of the total disintegration of an initial dendritic structure. The influence of an initial, transient solidification structure on the final solidification structure is demonstrated here for the first time in a metallic system. I) EXPERIMENTAL The technique of using a transparent flux to maintain an optically clean metal surface during solidification has been described by us elsewhere.* The

Jan 1, 1968

By Edward L. Beutner, Robert M. Crump

Benson Mines low-grade iron ore reserve is a replacement deposit within the Grenville gneisses of the Adirondacks. The average grade of the crude ore is about 23 per cent iron. The iron minerals are principally magnetite and hematite disseminated throughout the gneisses as discrete grains about 1 mm in size. Both the ores that are beneficiated by magnetic means and the non-magnetic ores that are treated by a gravity method of concentration are found in stratigraphically different positions but are mined from one open pit, which is about 2.5 miles long and 800 feet wide and are treated separately. The gneisses are described and named according to the distinctive mineralogy of each. Recognition of the gneissic types permits the interpretation of the structure as a northward-plunging syncline overturned to the west. A large subsidiary anticline-syncline complex occurs on the east limb of the major syncline. Iron minerals in sufficient quantity to be considered ore are confined to areas where the footwall rock has been overturned to become the hanging wall.

Jan 1, 1968

By W. E. MacDonald

This paper relates the story of 100 years of mining in the Harbour Seam at the Princess Colliery, Sydney Mines, Nova Scotia. Several interesting anecdotes are included along with the discussion of the evolution of coal mining methods in the area. Finally, some of the recently introduced equipment at Princess Colliery is described, and prospects for the future of the industry are outlined.

Jan 1, 1968

By Leonid V. Azároff, H. N. Murty

In the course of investigating the soft X-ray absorption spectra of Ni-A1 alloys, Das and ~zfiroff' observed an anomalous brittleness in solid solutions containing 3 to 5 at. pct Al. The brittle alloys also had anomalously larger lattice constants' and the fine structure at the nickel K edge of an alloy containing 3.96 at. pct A1 unexpectedly resembled that of NiA1 more closely than that of a solid solution containing 5.51 at. pct Al. This led them to suggest the possibility that short-range ordering was produced during the homogenization anneal to which each specimen was subjected, similar to that observed in dilute solutions of vanadium and of chromium in nickel: as the principal cause of embrittlement. It was decided to repeat the above measurements on several alloys in this composition range in order to test the above hypothesis and to establish the effect of heat treatment on the alloys' properties. Three solid solutions in this range were prepared containing, respectively, 3.16, 4.00, and 4.54 at. pct Al, in addition to alloys containing 6 and 9 pct. All samples were annealed in vacuum at 1800°F for 100 hr and then furnace-cooled to room temperature, as in the original study. The lattice constants of these alloys are shown by open circles in Fig. 1 and can be seen to fit quite closely the curve established by the previously measured values, indicated by solid circles. (The experimental errors are of the order of the size of the circles, +o.oo~R.) The three alloys containing 3 to 5 at. pct A1 were found to be quite brittle, as previously reported. In order to test the possibility of ordering, these three solid solutions were again heated to 1800°F and, following a few hours at that temperature, were quenched directly to room temperature. All three alloys lost their brittleness. In order to verify the proposed ordering hypothesis, it was decided to subject each sample to several cycles of quenching and annealing (disordering and ordering). After some experimentation, it was established that reproducible results could be obtained by anneal-

Jan 1, 1968

By C. E. Gregor

Current modern trends in mining show that hoisting shafts are being expected to fulfill an important ventilation function. However, where rigid guides and supporting structures are mandatory, ventilating power costs will be high, unless the transverse structures (shaft sets) are streamlined. In the complex configurations of hoisting shaft furniture patterns, either for original design purposes, or for the adjustment of an existing shaft, a useful degree of aerodynamic optimization, by reduction of overall resistance, can only be effectively evaluated by model studies in a special purpose wind tunnel, as described herein. The author has shown that, in one particular case, an annual power cost saving of more than $50,000 was indicated, mainly by the selection of buntons and dividers of improved aerodynamic profile. Mining companies are now realizing the advantages that can accrue through proper attention to the aerodynamic aspects of mine shaft design. With progressive demands of civilization for an ever greater supply of coal and metals, and with greater depths of working, higher rates of extraction, advanced degrees of mechanization, and improved standards of environmental health and work comfort, shaft design is becoming an extremely important aspect of mining operations. In addition, because the cost of sinking, equipping, maintaining, and operating a mine shaft is continually increasing, there is a greater incentive to use a shaft for the maximum duty, consistent with economy. The current natural tendency is therefore to sink multi-purpose shafts, to install as much equipment as is safely and effectively possible to operate; and then, over and above all these functions, to use the shaft to its maximum possible ventilating capacity, as a major, or auxiliary, airway. Clearly, this latter additional function can only be employed at a significant cost, since the most economic operating airways are smooth-lined and devoid of internal rigid furniture. It is true that hoisting functions can be carried out in such shafts if rope guides are used, but only under restricted conditions. Where a manway must be provided, fixed guides and supporting structures are mandatory, and ventilation costs become accentuated. It is generally recognized that the prime element of cost in ventilating a mine can be represented by the power required to drive the fan unit. It is also known that the largest component of total mine resistance is that of the downcast shaft, where this shaft is equipped with rigid guides for hoisting purposes. The pressure loss varies directly as the resistance of the shaft, in accordance with a modification of the Atkinson equation p = RQ2/3600. Furthermore, the air horsepower drawn is given by the equation AHP = (p x 0/33000. Therefore, the power required to drive the fan unit varies as the resistance of the shaft and the cube of the air quantity. Clearly, if Q is a specified minimum, then the only way to minimize the pressure loss (and the power costs) is to reduce the shaft resistance R. (See Table I for a list of symbols.) The resistance to airflow of a shaft equipped with rigid guides and supporting structural sets consists of two components which, for the sake of analytical simplicity, can be regarded as additive. 1) Frictional resistance, represented by the viscous frictional forces within the boundary layer, as air flows along the surfaces of the walls and the periphery of the vertical elements (guides, pipes, cables, ropes, etc.) of the furniture. The friction loss can be readily calculated by the Atkinson equation, after selection of a suitable value for the friction factor K from the McElroy compilation.' KxLxO xQ2 5.2 xA3 Friction loss can be minimized by lining the shaft walls (particularly if of circular or elliptical cross-section) with a smooth continuous lining of monolithic concrete.

Jan 1, 1968

By Peter R. Morris

The effecl of preferred orienlation on X-vay dzffvaction measurements of retained austenzte was investigated for four precipitation-hardening staznless steels in sheet form. A method is preserzted for estimating the ervor in measurement associated with a given samplirig direction. The method was used to select an "optimum" sampling direclion in order to minimize errors in measurement due to preferred orientation. hleasuremenls of retained austenite content employing lhe proposed sampling direction are conzpaved to measuretnents enzploying the more commonly used normal direclion for a series of sawzples. THE first application of X-ray diffraction to the measurement of retained austenite in steels is due to Sekito, 1 who employed a photographic technique in which the (111) reflection from a thin strip of gold affixed to a cylindrical sample was employed as a standard. Averbach 2 introduced the "direct comparison" method in which the ratios of observed to calculated random intensity are assumed proportional to the austenite and/or martensite contents. Averbach's work forms the basis of most subsequent X-ray diffraction methods for the determination of retained austenite. Subsequent improvements are due to: Averbach and Cohen,3 who employed a sodium chloride crystal to monochromate cobalt radiation; Averbach et a1.,4 who introduced a bent sodium chloride monochromator; Mager,' who used a bent quartz crystal to monochromate chromium radiation ; Littmam, who first used a geiger counter diffractometer for this purpose; Beu and Beu and Koistinen, 11,12 who studied effects of absorption factor, surface preparation, sample geometry, integrated intensity vs peak height, choice of radiation, monochromator, and filter. The possibility of errors in measured values due to orientation effects was noted by Miller,13 who suggested examination of a surface other than the plane of rolling. Lopata and Kula 14 have developed an experimental technique in which the preferred orientation is measured in each sample. They illustrated the method for a sample containing 42 pct retained austenite. Application of their technique to the 1 to 15 pct range typical for the precipitation-hardening stainless steels does not appear feasible. EXPERIMENTAL PROCEDURE The nominal compositions of the precipitation-hardening stainless steels investigated are listed in Table I. Ingots were solution-treated, hot-rolled to approximately 0.2 in., and reduced to 0.050 in. by a suc- cession of cold rolling and annealing operations. After this treatment the 17-4PH sample was in the marten-sitic condition, while the 17-7PH, PH 14-8Mo, and PH 15-7Mo samples were in the austenitic condition. Samples of 17-7PH and PH 15-7Mo steels in the mar-tensitic condition were obtained by heating to 1750'F for 10 min and holding at -100°F for 8 hr. A sample of PH 14-8Mo steel in the martensitic condition was obtained by heating to 1700°F for 1 hr and holding at -100°F for 8 hr, followed by aging at 950" for 1 hr. POLE FIGURE DETERMINATIONS Samples were thinned to 0.003 to 0.005 in. by etching in a solution containing 250 ml reagent-grade phosphoric acid (85 to 87 pct H3PO4), 250 ml technical-grade hydrogen peroxide (30 to 35 pct H 2 O 2), and 50 to 100 ml reagent-grade hydrochloric acid (37 to 38 pct HCl). The specimens were placed in an "integrating" sample holder which provided a 1-in. oscillation in the plane of the sample. The diffractometer was aligned to measure the intensity diffracted by planes of the particular {hkl} type being studied. The sample was Set for a given latitude angle, a, measured from the plane of the sheet, and diffracted intensity recorded as the longitude angle, 0, measured in the plane of the sheet from the rolling direction, was increased from 0 to 360 deg. After a 360-deg scan of B, a was incremented by 5 deg, and the process repeated. Random standards obtained by spraying suspensions of powdered iron (bcc structure) and nickel (fcc structure) in lacquer were used to correct observed intensities for absorption and geometrical effects. Zirconium-filtered molybdenum radiation was used to determine the transmission regions of the (111) (0to 45 deg), (200) (0 to 60 deg), and (220) (0 to 45 deg) austenite and (110) (0 to 45 deg), (200) (0 to 50 deg), and (211) (0 to 35 deg) martensite pole figures. Vanadium-filtered chromium radiation was used to

Jan 1, 1968

Unfortunate occurrences resulting in injuries, loss of life, and destruction of property by explosion, fire, and other mishaps during shaft sinking focused the attention of the Bureau of Mines on the need for safety standards For such operations. Information Circular 7810 was published to meet that need. The current revision updates and replaces IC 7810. Several States have some rules and regulations applicable to local conditions, and several Bureau publications (including some now out of print) cover the hazards that may be encountered in shaft sinking. Certain requirements of the Federal Mine Safety Code and Federal Coal Mine Safety Act may be applied, but there are no definite, uniform standards that will guide those desiring to sink a shaft safely and bring about uniform safety inspections.

Jan 1, 1968

By O. D. Gonzalez

ThIS communication presents the results of a determination of the permeabilities of hydrogen and deuterium in a iron from 360° to 560°C. Recently Heu-mann and primas' have given values of the diffusivity and solubility in a iron of the two isotopes from which the permeability can be calculated. The work reported in the present communication, however, is a direct measurement of the rate of permeation of the isotopes through an identical iron specimen under the same conditions, so that systematic errors can be minimized in the calculation of the ratio of the permeabilities—the value which is usually of main importance in establishing limits for isotopic differences in diffusive processes. Experimentally the procedure used was the usual one: a steady-state flow of gas produced by a pressure difference across an iron membrane was observed as the pressure rise with time in a previously evacuated, calibrated volume connected to the outlet side of the membrane, while a constant pressure of gas was maintained on the opposite inlet side. The membrane was a cylindrical tube 9.38 cm long, 0.730 cm inside diam, 0.187 cm wall thickness, fabricated of 99.95 pct vacuum-melted National Research Corp. iron (less than 0.003 pct C). One end was sealed by a heliarc-welded iron (99.95 pctj lid of 0.147 cm thickness; the other end of the tube was welded to a 304 stainless-steel tube (0.318 cm ID and 0.318 cm wall) which connects to a vacuum system and to the calibrated volume including a dibutylphthalate manometer. The temperature of the iron membrane was maintained constant to ±0.l°C and was measured with an iron-constantan thermocouple which was calibrated against a standard Pt/Pt-Rh thermocouple: the temperature variation along the length of the membrane did not exceed ±0.5°C. Hydrogen was allowed to pass through the membrane assembly for 72 hr at 615°C before permeability measurements were begun. The system was tested at temperature before and after the experiments by a substitution of helium for hydrogen in the inlet side; under these conditions the pressure rise observed in the outlet side was negligible at all times. The gases used for the permeability measurements were 99.95 pct Matheson prepurified H2 and 99.7 pct D2 (0.3 pct HD) from the Isomet Corp. The gases were dried with liquid N2 before use. In Fig. 1 the logarithms of observed flows, jt, for a pressure difference of 73.4 cm Hg are plotted against T-1 Each point in Fig. 1 represents the slope determined by a least-square evaluation of a plot of the pressure in the outlet side of the membrane against time, including at least two separate sets of observations. Each point in the figure has an uncertainty of ±0.6 pct arising from the experimental uncertainty in the pressure and time measurements. The standard deviation of the observed pressures from the straight lines in all cases is less than the experimental precision of the measurements. The observed flow, jt, includes a small but not negligible flow through the stainless-steel connection.

Jan 1, 1968

By C. I. Pierce

The Bureau of Mines conducted laboratory tests to determine if ultrasonic energy could reduce either the residual water or oil content of petroleum reservoir-rock samples from Appalachian area oilfields. Brine-saturated core samples were flooded with oil to residual brine saturation and subjected to 20 kilocycles per second ultrasonic energy. Then they were flooded with brine to residual oil saturation and again subjected to ultrasonic energy. Additional water displaced as a result of the application of ultrasonic energy to the flow system ranged from 0 to 4.3 percent of the original brine and averaged 1.9 percent. The increase in oil recovery as a result of the ultrasonic energy ranged from 0 to 9.0 percent of the original oil and averaged 3.1 percent. On the basis of the tests, it appears that 20-kcps acoustic waves would not have field application for oil recovery.

Jan 1, 1968

By O. B. Bucklen, P. G. Meikle

INTRODUCTION The trend in the coal industry for many years has been to make every- thing "bigger and faster." This also held true for loading and storage facilities. Where once a million ton per year mine was rare, three to five million ton per year mines are not uncommon today in the bituminous industry. This greatly increased production, made possible through mechanization, required greatly improved loading facilities just to get the coal away from the mine. Also, there is a trend toward combining production from more than one mine and cleaning it in a single preparation plant. In addition to increased loading capacity, this frequently necessitates raw coal storage and blending facilities. The development of the unit train with its attendant economics, more than any other factor, has contributed to the widespread construction of storage and high-speed loading facilities. In the export market, the construction of ever larger coal colliers has contributed to a need for faster and larger loading facilities. In this climate of rapidly changing technology, any written account is faced with the possibility of obsolescence before its appearance. Thus, this chapter seeks to define the common and current practice in coal loading and storage facilities with the full knowledge that this practice is an ever-moving target. FUNDAMENTALS OF COAL STORAGE Storage of coal is becoming an increasingly important part of coal handling systems at mines, particularly since the advent of the unit train concept in transportation. In order to take advantage of reduced transportation rates on trainload shipments of coal offered by unit train movement, operators have found that storage is an economic necessity. In unit train practice large predetermined quantities must be loaded in relatively short periods of time as opposed to conventional practice where coal is loaded at a speed dependent on the production capacity of the mine and/or the cleaning capacity of the preparation plant. Two surveys of storage practices at mines reveal several objectives for storage.1, 2 Raw and/or clean coal storage is generally practiced in order to accomplish one, or a combination, of the following objectives: 1. To improve plant efficiency by distributing plant feed over the entire operating time, or to allow a preparation rate different from the production rate. 2. To limit interruptions of supply, ie, allow mine and plant to function independently with delays in one not affecting the operation of the other.

Jan 1, 1968

By Frederick C. Moore

This paper describes the original planning which actually resulted in the opening of a new aggregate plant located in central New York State. This plant, which is now named the Skaneateles Plant of The General Crushed Stone Company is unique in that the plant itself is a departure not only in design but in concept of operation from the normal aggregate plant the company has operated in the past. Whether or not the concepts which resulted in the Skaneateles Plant are economically feasible remain to be proven by the next few years of operation. By way of background data about our company which will help set the stage for this presentation, we currently operate seventeen stone quarries in the states of New York, Pennsylvania and Virginia. These quarries range in size from 200,000 tons per year to 1,500,000 tons per year with a total annual stone production of approximately 7,500,000 tons. We also produce about 1,250,000 tons of sand and gravel at six sand and gravel plants, 300,000 cubic yards of ready mix concrete, 1,500,000 tons of bituminous concrete, aglime and other minor construction materials. In many cases we are our own best customer consuming a large percentage of the total production of our own aggregates in our various ready mix and blacktop plants. Up to the concept of the Skaneateles Plant our operating facilities have been of the permanent type as opposed to the moveable or portable type plant. The steps involved in the case history of Skaneateles will begin with the basic economic requirements, market research, geologic surveys, land acquisition, zoning and financing and carry through to the final design and construction. We will attempt to show what some of the problems were, how we interpretted them and how we proceeded to solve them. The current results are apparent and can be analysed. The success of the total concepts of the Skaneateles Plant remains for future analysis.

Jan 1, 1968

By Robert D. Pehlke, Kazuhisa Okajima

The activity of zinc in dilute liquid lead alloys containing small additions of silver and gold has been measured using a multielectrode galvanic cell with a fused chloride salt electrolyte. The range of temperatures studied in the Pb-Zn-Ag system was 550" to 670°C and in the Pb-Zn-Au system was 680" to 800°C. The interaction parameters between zinc and the precious metals in the respective temperature ranges are ThE lead-rich corners of the Pb-Zn-Ag and Pb-Zn-Au ternary systems are of considerable industrial importance. The use of zinc additions for the desilvering The results of this investigation have Provided a senzi-quantitative determination of the liquidus phase boundaries in the lead-rich corner of these ternary diagrams. of liquid lead either by the Parkes process or by the more recent Williams continuous process is an important refining phase of lead production.1 Several in-ve~ti~ations~-~ have been carried out on the Pb-Zn-Ag system with the hope of improving the efficiency of refining lead in this manner. The addition of zinc also provides a means for separating gold from lead. Since gold is eliminated more easily than silver, a two-stage removal of gold and silver is possible.8'7 The thermodynamic interactions between zinc and these precious metals in dilute solution in liquid lead

Jan 1, 1968

By S. Nakajima, H. Okazaki

Quantitatiue studies of the deformation texture in drawn tungsten wives were made by the X-vay dif-fractottletetr. Experimental results show that the diffraction Intensities are equal to tilose pvedicted from the (1 10). fiber lexlure but the angxla), spreads of. diffraction peaks in the pole distribution curres are different for different diffraction planes and directions. For this reason a modified (110) fiber lextuve model, in which a kind of anisotropy is assumed, is proposed to explain the results. According to this model the poles lying on a line directing front the (110) to the (110) poles in the (1 10) standard stereograpllic projection should show spreads which are different from those lyitlg on a line directing from the (001) to the (001) poles, which is confirmed by the experiments. The anisolvopy and the spveads of the pole positions are large at the outer part of the wires and decrease gradually lowards the inside of the wire. The possibilily of occurrence of such anisolropy in irrelals with fcc stvuctures is discltssed. THE deformation texture of drawn tungsten wires has been assumed by different investigators to be the simple ( 110) fiber texture.' Recently, however, Leber2,3 has shown that a swaged tungsten rod has a cylindrical texture. It changes gradually to the (110) fiber texture by drawing through dies. However, even after drawing to 0.25 mm in diam, the cylindrical texture can still be found in wires together with the (110) fiber texture. This was deduced from the pole figures obtained from the longitudinal section of these wires. Use was made also of quantitative measurements of the pole distribution curves. Leber stated that the angular spread of the pole distribution curves (henceforward called dispersions) are quite different for (400) 45 deg and (400) 90 deg: the former is always larger than the latter. This inequality is accompanied by deviations of the diffraction intensities from the theoretical values for the ( 110) fiber texture. Bhandary and cullity4 have reported similar results on iron wire and explained them by assuming a cylindrical texture. Both Leber3 and Bhandary4 used only the results of the (400) reflection for the determination of the dispersion. The pole figures found by Leber3 and by Rieck5 are largely different. The model given by Leber to explain the effects is in the authors' opinion in some respects unsatisfactory, especially if one looks at other than the (400) reflections. Intensities and dispersions of diffraction peaks are conclusive factors for the determination of the fine structure in wire textures. For this reason we studied them extensively to come to a model which is more suitable to fit the facts. In the following, after giving the experimental set-up, we report about measurements of X-ray diffraction on drawn tungsten wires. Different models to describe the experimental results will be discussed. EXPERIMENTAL GO-SiO2-A12O3 doped tungsten wires drawn to 0.18 mm in diam were used for the measurements. The wires were chemically etched to various diameters down to 0.03 mm. Measurements were carried out for the different wires in order to determine the dependence of the texture on the radius. The wires were cut to pieces of 10 mm length and fixed with paste closely against each other on a flat, polished glass plate. Parallelism of the wires with the surface of the glass plate should be adequate. For the diffraction studies three different X-ray sources were applied, respectively, giving the CuK,, FeK,, and FeKp emission. The measurements were carried out with a diffrac-tometer with a GM counter. The latter was fixed to a certain diffraction angle 20hkl and the diffraction intensity was recorded as a function of the angle of rotation of the specimen around the axis, lying in the specimen surface and perpendicular to the wire axis, as shown in Fig. 1. Measurements were also done with the detector at angles slightly deviating from the diffraction maxima The measured intensities in this case were taken to be equal to the background level. The deviations were chosen as small as possible but large enough to eliminate the influence of the diffraction maxima. The useful range of the rotation angle x of the specimen is generally limited by the wavelength of the X-rays. We have: where and cp is the angle between the wire axis and the normal of the diffraction plane. Intensity measurements were made to find the necessary corrections for counting loss of the GM counter and for distortion resulting from such effects as absorption of X-rays and from inclination of the reflection plane under study with respect to the surface of the specimen. The counting loss was esti-

Jan 1, 1968

By C. D. Thurmond

Jan 1, 1968

By J. C. Swartz

Measurements of the effect of precipitation stresses on the solubility of cementite (Fe3C) precipitates in a iron are reported. Solubilities were determined from measurements of the Snoek relaxation due to interstitial carbon after quenching from various equilibrium treatments. Stress-free precipitates were obtained by a spheroidizing treatment of vacuum-melted Fe 0.06 wt pet C. Subsequent equilibration treatments were designed to suppress nucleation of other precipitates. The results for stress-free cementite give a heat of solution of 14.8 i 0.2 keal per mole and an entropy change of 1.1 i 0.2 eu in the temperature range 400" to 715°C. Comparison with previous data indicates that the heat of solution increases about 6 keal per mole as temperature increases from 700" to 1000°C. Data on self-stressed cementite in quench-aged specimens of Fe 0.013 wt pet C indicate 1) an apparent heat of solution of 12.1 i 0.4 keal per mole in the range 280" to 690°C, 2) a strain energy of- 1.1 keal per mole Fe3C accompanying precipitation at 280°C, and 3') a gradual decrease in the strain energy of precipitation with increasing equilibration temperature. In com-parison with 2 and 3 the strain energy calculated for an isotropic model is 1.7 keal per mole Fe3C. The lower values obtained from the experiment indicated substantial stress velaxation by dislocation motion. WHEN a supersaturated solution of carbon in a iron is aged at temperatures in the range 200o to 700oC, the carbon clusters by interstitial diffusion and forms cementite (Fe3C) precipitate particles. Unstressed cementite has a volume per iron atom 9 pet higher than that of a iron;' hence, cementite precipitate particles are usually under pressure from the iron matrix. The pressure would tend to increase the solubility of cementite in iron.' This report describes anelastic measurements of the solubilities of self-stressed and stress-free cementite in a iron. Previous determinations of the cementite solubility are summarized in Table I. The method of cementite formation for each reference was studied to ascertain the state of stress of the cementite. The results judged to be for stress-free and stressed cementite are distinguished in the table. In the next section an estimate of the stress effect is obtained which is clearly too small to account for the large difference between the previous results in parts A and B of the table. THEORETICAL Let AGO be the standard free-energy change of the reaction Fe3C (eem.) = 3Fe (a) + C (in a) [1] in the absence of stresses. Since cementite precipitates appear to be rather pure10 and the carbon is so dilute in the iron,8 the cementite and iron of Eq. [ I] for the stress-free case have essentially unit activities and the activity of carbon equals its atom fraction xoC Then the stress-free equilibrium is expressed by RT In XoC = -?GO 121 To first approximation the change in the chemical potential of carbon due to the precipitation stresses equals the elastic strain energy W accompanying precipitation of a mole of cementite.2 Hence, in the presence of the precipitation stresses the equilibrium is described by RT In x sq = -?G° + W [3] where xsC is the mole fraction of dissolved carbon in the stressed case. An approximate value of W can be obtained from analysis of the inclusion problem in elasticity theory. The inclusion is a small portion of the matrix phase which has suffered a transformation while still imbedded in the matrix. In the absence of the constraint of the matrix the transformation would be equivalent to a uniform dilational strain eT. Both the matrix (a) phase and inclusion (0) phase are assumed to be homogeneous, isotropic materials. When the a and 0 phases have the same elastic moduli, which is approximately true for iron and cementite,11 the total strain energy per mole ß is12 2µVß(eT)2(3 +4 µx)-I [4]

Jan 1, 1968

By O. D. Sherby, J. L. Lytton, C. R. Barrett

Randomly oriented polycryslalline copper of 99.995 pcl was tested in tension at temperatures of 626o, 496o, and 406o. The gvain-size mnge investigated was from 0.03 to 0.7 mm. Grain sizes were produced by two techniques: 1) varying the amount of prior cold work and the amealing time at constant annealing temperature so as to obtain various vecrystallized grain sizes with minimum grain growth, and 4 holding the prior cold work constant while varying the annealing time or temperature so as to obtain varying grain sizes by grain growth. Polycrystalline samples (grain size of 0.03 mm) with a strong. [001](100) texture were also studied. The relationship between the steady-state creep rate, Es, and pain size was found to be the same indepentent of the technique used to prepare the various grain sizes. For specimens with grain diameters above about 0.1 mm ea zuas esse)ztiallj~ independent of grain size, while for smaller grain diameters Cs increased slightly with decreasing grain size. Strongly textured polycrystalline copper, which contained low-angle grain boundaries, exhibited steady-state creep rates that were slightly lower than those observed in randomly oriented copper, of the same gain size. The results are explained by conside?%ng- the contribution of grain boundary shearing to the total strain and the effect of grain size on the resulting creep substructure. EXPERIMENTAL observations concerning the influence of grain size on steady-state creep rates are varied and oftentimes conflicting. Numerous early investigators found that an increase in the grain size resulted in a decrease in the high-temperature steady-state creep rate, i,.'-" Other workers have foundthat ef decreases with increasing grain size up to some optimum grain size and then increases with a further increase in grain size.'- '' It has been suggested that es, decreases with an increase in grain size only because the range of grain sizes studied normally lies to the left of the grain size for optimum creep resistance. However, sherbyl2 and Feltham and his co-worker13, 14 have found that even for small grain sizes 2, does not always decrease with an increase in grain diameter but may be proportional to the square of the grain diameter. A possible explanation for the different creep rate-grain size relationships which have been observed is that in most experimental studies different grain sizes have been prepared by annealing at various temperatures. For metals in which the impurity concentration is high (greater than about 0.1 at. pct) this type of

Jan 1, 1968

By S. Jana, C. M. Wayman

The reverse transformation of bcc martensite to the fcc phase was studied in an Fe-33.95 wl pct Ni alloy by nzeans oj dilatometry, melallography, and electron microscopy. Upon "slozc" heating (-1°C per min) length cJmnge us temperature plots showed u gradual contracLion over the temperature range 200" to 280"C ,followed by a more abrupt contraction beginning a1 -280°C. Howet,ev, zchen the heating rate was increased -4°C per tnin, no gradual contraction was observed and only the abrupt contraction starting at -2BO"C was found. Thus on slower heating- the AS "temperature" for the subject alloy, unlike the MS temperature, is better defined as a range of temperatures. Both optical and transmissiorl electron microscope observations showed that some of the martensite plates exizibited a partial loss of transformation twins during reversal. The midvib region of the martensite plates disappeaved relatively early duirng the reversal. Metallographic observations slowed that the earliest detectable stage of the rezlerse tvansforrvration begins (axd Moues inulardly) at The Martensens i te - parent interface. At higher temperatirres, the. formation of martensitically reversed jcc plates within the bcc martensite plales was observed. It is concluded that the reverse transformation consists of a diffusion less process (martensitic); but this is ps-obably aided by a prior or simultaneous dijjusiorz-comltvolled process, at leasl in the case of slower heat-ing' experiments. ALTHOUGH numerous investigations have dealt with the parent-to-martensite ("forward") transformation (fcc — bcc) in Fe-Ni alloys, comparatively little is reported on the ("reverse7') martensite-to-parent transformation.'-4 Even though such reverse transformations have been studied in detail in some nonferrous systems, one of the difficulties of studying the reverse transformation in most ferrous mar-tensites is that the martensite decomposes by tempering during heating. However, carbonless Fe-Ni alloys do not exhibit this difficulty since the transformation in these alloys is completely reversible. The present investigation represents an attempt to shed more light on the nature and mechanism of the martensite-to-parent transformation. 1) EXPERIMENTAL PROCEDURE 1.1) Alloy Prepatation. Fe-Ni alloys of compositions near 34 wt pct Ni were prepared from zone-refined iron (99.994 wt pct Fe) and high-purity nickel (99.999 wt pct Ni) by induction melting in recrystallized alumina crucibles in an argon atmosphere, with prior vacuum evacuation to 10"3 mm Hg. The alloys were homogenized by induction stirring in the molten state for 5 min. After solidification, the alloys were further homogenized in evacuated quartz capsules for 96 hr at 1230°C. 1.2) Dilatometry. Slices of the ingot were hot-forged (750°C in air) into approximate rod form and these specimens were then hot-swaged (750°C in air) into long cylindrical rods 0.55 mm diam. From the rods, specimens about 1 in. long were cut. These were then vacuum-annealed for 24 hr at 1200°C, cooled to room temperature, and subsequently transformed to martensite in liquid nitrogen (whereby about 40 pct transformation was obtained). Dilatation measurements were made by observing length changes in a vacuum dilatometer with an externally mounted LVDT sensing element. 1. 3) Preparation of Electron Microscope Specimens. Slices of the ingots were cold-rolled (with intermediate vacuum anneals) to -0.020 in. Out of these rolled sheets, specimens (about 1 by 1 in.) were cut. These were then vacuum-annealed, transformed to martensite by cooling in liquid nitrogen, and subsequently heated from room temperature to various temperatures to effect either partial or complete reverse transformation. These specimens were then chemically polished to 0.002 in. in l:l HsOz (30 pct) and &PO4 (85 pct) solution, and thinned to electron transparency in an electrolyte consisting of 150 g CraOs, 750 ml glacial acetic acid, and 30 ml ~~0.~ Observations were made with a 100-kv Hitachi HU-11 electron microscope equipped with an HK-2A tilting device. 1.4) Optical Microscopy. Metallographic observations were made with a Leitz MM5 metallograph on the same 0.020-in. sheet specimens as were used for electron microscopy and on bulk specimens which were 0.2 in. or more on a side. The chemical thinning solution when cooled below 20°C also served as an etchant for this alloy. Observations of surface relief were made with a Zeiss interference microscope employing a Thallium light source of wavelength 0.54 p. Specimens for interference studies were prepared by two-stage polishing on Buehler vibromet polishers using 0.3 and 0.05 p alumina abrasives. 2) EXPERIMENTAL RESULTS 2.1) Comparison of the MS,AS, and Af Tempera-tures wTth Previous Re sults. The AS aLd Af tempera -tures of several Fe-Ni alloys were determined dila-tometrically. The MS temperatures of the same alloys were determined by continuously lowering the temperature using a mixture of isopentane and liquid nitrogen and observing the highest temperature at which a prepolished specimen showed surface upheavals. For the present the As temperature is defined as the temperature at which an abrupt decrease in length occurs in the dilatation plot. The Ms,As7 and A determinations in the present investigation and those of Kaufman

Jan 1, 1968