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By R. H. Cox, A. S. Allen, James Paone

The southwestern Illinois communities of Belleville and Maryville lie within the greater metropolitan area surrounding St. Louis. Missouri. They also lie within that part of the Illinois coal basin where the Number 6 coalbed has been mined for more than a century. About half the coal was left as pillars to support the ground surface. Years later, however, damaging movements are affecting buildings, streets, and public utilities in some areas. They are generally believed to be related to abandoned mine workings. The threat of continued or increasing incidence of damage raises the need to explore other subsidence-control measures for protecting affected areas with high population density. Because of experience gained in a subsidence-control program of backfilling abandoned coal mines in the Applachian region and in Rock Springs, Wyoming, the Bureau of Mines was called upon to investigate the subsidence occurrences at Belleville and Maryville, and recommend protective measures. Funds ware appropriated for the Bureau to initiate subsidence-control projects at two residential sites in Belleville and one in Maryville. Subsurface investigation of the sites by diamond core drilling revealed two conditions that differ from those encountered at most sites of previous subsidence-control projects. The mine workings were found to be dry and the mine floor consisted of soft underclay which characteristically loses strength with increase of moisture. It had been anticipated that water would have percolated into the mine workings at one .or more of the sites through cracks resulting from subsidence. Under such conditions Bureau engineers believed that injection of mine waste by the pumped; slurry technique3 would provide support and stabilize any movements initiated by the softening of the clay. With discovery that the underclay deposits at the three sites have apparently not been exposed to water since the mines were operating, hydraulic backfilling of any type was considered inadvisable on the basis of present knowledge. To avoid introducing water, a portable pneumatic system is being devised for injecting minus 0.01 27 m (1/2 in.) mine waste into the mine workings. Machines for pneumatic backfilling have been used in Europe not only for subsidence protection but also for strata control, for reducing spontaneous combustion and methane accumulation, and as a means of waste disposal. The Bureau experimented with a pneumatic machine in the Northern anthracite field of Pennsylvania in the 1950's. Previously pneumatic machines have been installed in active mine workings discharging from horizontal pipelines which conveyed air- borne material into rooms to be filled. In the present adaptation to abandoned mines, the machine and air compressor will be operating at the surface, to impel material vertically down injection boreholes with sufficient air pressure to disperse fill material laterally in mine workings at the base of injection holes. Large diameter access and ventilation boreholes will be provided at one site for entry into mine workings to observe backfilling progress. The Belleville and Maryville projects are part of the Mined Land Demonstration Program of the Bureau of Mines. The Illinois State Geological Survey and Department of Mines and Minerals are furnishing technical support.

Jan 1, 1979

MORE than 5000 miners and suppliers descended upon Denver to make the American Mining Congress' four-day metal mining show one of the most extravagant equipment displays ever assembled in one place at one time. The most recent developments in equipment for mining, milling, and processing ore were shown by the 146 exhibitors at Denver's new City Auditorium which covers 57,000 sq ft of floor space. Other displays were placed in the open air opposite the auditorium site. Registration desks were opened Sunday, Sept. 21. A field trip to the Colorado School of Mines at Golden was the featured activity of the day. Official opening of the show took place on Monday, and presided over by Howard I. Young, president of American Zinc, Lead & Smelting Co.; Otto Herres, vice president, Combined Metals Reduction Co.; William J. Coulter, vice president, Climax Molybdenum Co.; Charles B. Stainback, Westinghouse Electric Corp.; and Merrill E. Shoup, president, Golden Cycle Corp. Convention welcoming addresses were delivered by a representative of Mayor James Q. Newton, of Denver, and Gov. Daniel V. Thorton of Colorado. Following the formal opening ceremonies a round table discussion dealt with the "Paley Commission Report" formally called Resources for Freedom. Participating in the panel were: Arthur H. Bunker and George R. Brown, members of the Paley commission; H. I. Young, president of the American Mining Congress; Horace M. Albright, president of U. S. Potash Co.; Evan Just, vice president, Cyprus Mines Corp.; Donald H. McLaughlin, president, Homestake Mining Co.; E. H. Snyder, president Combined Metals Reduction Co.; Simon D. Strauss, vice president, American Smelting & Refining Co.; Sen. H. C. Dworshak (R.-Idaho) ; Ira B. Joralemon, consulting engineer; Jess Larson, De fense Materials Procurement Agency; and Andrew Fletcher, president of St. Joseph Lead Co. The panel discussed the report for six hours, adding a great deal of information to the already voluminous amount which has been gathered concerning it. Three objections to the report frequently mentioned were: 1-the multilateral contract; 2-international buffer stocks; 3-international buffer stocks combined with limited quota arrangements. Points on which the panel commended the report were its recommendations for acceleration of topographic and geologic mapping of the United States and Alaska; recognition of the principle of percentage depletion for metals and minerals; and advocation of removal of the present limitations on the expensing of exploration costs applicable to minerals. Technical sessions were held throughout the four days of the meeting. Included in the program were: Progress in Mechanication; Small Mines; Public Lands; Open Pit Mining; Manpower-Labor Relations; Shaft Sinking; Roof Support; Taxation, Gold, Silver and Monetary Policy; Advances in Mill Practices; Special Conference on Strategic Materials; Uranium Mining-Atomic Energy; Prospecting and Exploration; New Metallurgical Processes; and Rock Breaking. About 45 papers and several panels were presented during technical sessions. Formal and informal social functions consumed the remaining time of the convention. Three locations were needed to handle the huge throng attending the Mining Jamboree Monday evening. The only other sponsored social function took place Thursday evening. A great many informal gatherings, chiefly convivial, were held in manufacturers' courtesy rooms-called wet stopes. Field trips included Cripple Creek, Pueblo, Climax -Leadville-Gilman, Colorado Plateau-Grand

Jan 1, 1952

By M. E. Wadsworth, P. H. Yu, C. K. Hansen

A study of the rate of dissc5lution of chalcopyrite (CuFeS2) in acidic solutions under oxygen overpressures was carried out by measuring the rate of formation of cupric ions in solution. Effects of temperature, oxygen partial pressure, surface area, and concentration of sulfuric acid were evaluated. A sized batch of chalcopyrite was leached in the temperature range of 125° to 175°C and in the pressure range of 75 to 400 psi of oxygen. In 0.5 N H2SO4 all products of reaction went into solution except for trace amounts of elemental sulfur. The dissolution of chalcopyrite followed linear kinetics and was essentially independent of hydrogen ion concentration for H2S04 concentrations between 0.2 and 0.5 N. The oxygen dependence indicated adsorption approaching limiting values with increasing oxygen pressure. The linear mechanism was explained in terms of steady-state adsorption of oxygen at the chalcopyrite surface followed by a surface reaction. The enthalpy of activation for adsorption of oxygen was found to be approximately 33 kcal per mole. An activation enthalpy of approximately 9 kcal per mole was observed for the surface reaction. Charge transfer reactions are not rate controlling in the process.

Jan 1, 1973

By Norman Brown, Victor V. Damiano

ThE present paper proposes a mechanism of dislocation multiplication at internal inclusions or cavities and presents experimental evidence of such sources in zinc. Using an etching technique recently described by Damiano, Tint, and Herman1 to study the three-dimensional aspects of dislocations in bulk zinc crystals, an investigation was made of helically shaped and closed-loop etch patterns found to be associated with inclusions. Crystals containing 0.1 pet Cd and grown from the melt were deformed slightly by bending and then aged at room temperature to precipitate cadmium at the dislocations. The crystals were cleaved along the (0001) plane and then etched with Gilman's2 etch. Crystals were continuously viewed on the (0001) plane while the etching was in progress and numerous helical and closed-loops etch patterns were continuously recorded as shown in the sequences printed directly from the cine film in Fig. l(a) and (6). These etch patterns are not to be confused with the etch patterns previously reported by Damiano and Herman3 which revealed dissolution spirals on the (0001) plane of high-purity zinc crystals. In the present case, precipitates arranged in the form of closed loops or helicies are progressively uncovered by etching after suitable aging of cadmium doped zinc crystals. Viewed with dark-field illumination as shown in Fig. 2, portions of a helical figure and subboundaries were revealed simultaneously. Continuous viewing while the etching was in progress revealed in Fig. 1(b) that the short line segments observed on single photomicrographs were in fact continuous and described a helix which had its terminus at an inclusion. The observations suggested that a dislocation once nucleated at the interface between the inclusion and matrix may act in such a way as to produce ad-

Jan 1, 1964

By Lawrence H. Van Vlack, Otto K. Riegger, Gerald I. Madden

The microstructural variations of periclase (MgO) in the presence of oxide liquids are examined under the steelmaking variables of: 1) temperature, 2) liquid composition, and 3) FeO additions under different oxidation levels. Attention is given to the distribution of the phases, both liquid and solid, and to the growth of individual crystalline grains. Silicate liquids penetrate more extensively between individual periclase grains than do liquids containing high percentages of Fe2O3 Higher MgO solubilities in the liquid and lower MgO contents of the solid favor more rapid grain growth. The presence of a second solid phase reduces the periclase grain growth rate and increases the amount of the solid-to-solid contact within the oxide microstructures at high temperatures. The service suitability of a refractory depends on many factors. Two are of major importance and include 1) the thermal resistance to melting, and 2) the mechanical resistance to loads at service temperatures. Neither is a simple consequence of the service temperatures because service conditions will alter compositions, produce partial melting, and induee phase changes. Consequently, the equilibrium phase relationships have been rather thoroughly studied and give a knowledge of the thermal resistance to melting, but do not give full information about the mechanical properties because two refractories with the same types and quantities of phase may have different microstructures. Although variations of microstructures with time, temperature, and composition have been subjects for extensive investigation in metals, only a limited amount of comparable microstructural work has been performed for refractory materials.' This study was an attempt to evaluate some of the consequences of service parameters upon the microstructures of refractories so that bases may be established for the analyzing of high temperature mechanical properties. Periclase (MgO) was chosen as the refractory oxide; variables included those which are encountered under steelmaking conditions such as 1) temperature, 2) liquid composition, and 3) FeO additions under various oxidation levels. Specific attention was given to the distribution of the phases, both liquid and solid, and to the growth of individual crystalline grains. The most closely related work on microstructures of polyphase materials is that of Van Vlack and Rieg-ger2 on the microstructure of magnesiowüstite [(Mg,Fe)O] in the presence of silica. In that work which pertained to solid solutions with less than 40 pct MgO, most of the quantitative work was performed on FeO microstructures. The chief conclusions concerning these relatively low-melting oxide solids were as follows: 1) the rate of crystalline grain growth is inversely proportional to the grain diameter, 2) grain growth proceeds more rapidly at higher temperatures but is slightly retarded by additional liquid content, and 3) a Silicate-containing liquid penetrates as a film between the individual magnesiowüstite grains independent of time, temperature, amount of liquid, or the MgO/ FeO ratio. The above observations are in contrast to prior work3 on the microstructure of silica in the presence of iron oxide-containing liquids where the liquid does not penetrate as a complete film between solid grains. The phase relationships for the compositions of the present work are shown in Fig. 1 which is a summary of the work of several investigators.4 Of importance is the fact that CaO forms a more stable structure with SiO2 and Al2O3 than do either MgO or FeO. The oxygen potential has little effect on periclase unless iron oxide is also present. The iron oxide is ferrous at moderately low oxygen levels, changing to ferric as the Oxygen potential is increased so the spinels, magnetite, and magesioferrite are formed.5 These two phases are relatively stable in air at steelmaking temperatures. I) EXPERIMENTAL PROCEDURE ractory were made with reagent grade Oxides. The magnesium oxide used was 99 pct MgO after ignition, and the iron oxide raw material had a minimum content of 99 pet Fe2O3. The CaO, SiO2, and A12O3 were also reagent grade raw materials. After mixing, the required compositions were pressed into pellets at a minimum pressure of 5000 psi to insure compaction of the raw materials and prevent excess void content. A silicon carbide element tube furnace was used with thermocouple control for sin-

Jan 1, 1963

By G. S. Hume

Production of petroleum and natural .gas increased in Canada in 1940 over the previous year. Alberta produced more than 97 per cent of the total Canadian production of 8,718,053 bbl. of oil, an increase for this province of nearly 12 per cent, whereas in Ontario and New Brunswick, where the production is relatively small, there was a slight decline. In Alberta the main producing field is Turner Valley, on the eastern edge of the foothills southwest of Calgary, and development continued in this field in 1940 with the completion of 36 wells, all of which obtained production. In the Red Coulce field, close to the International Boundary, near Coutts, no new wells were drilled and the seven producing wells showed a decline of 900 bbl. below the previous year. Also, in the Wainwright field of east central Alberta, four wells, yielding heavy crude oil, produced 4000 bbl. less oil than in 1939, owing possibly rather to discontinuous operation than to actual decline in potential yield. This decline was more than offset by production from a new field 40 miles northeast of Wainwright, at Borradaile, producing oil of 14" to I 5° A.P.1. There was a small increase in production during 1940 from the Del Bonita field, in southern Alberta, where the production is from two wells. The outstanding development of the year was the completion of Standard Oil Princess No. 2 well in the Steveville area, on the Plains 100 miles east of Calgary. This well was completed late in December with an initial flow1 of 520 bbl. of 26.3" A.P,I. oil, and 12,750 M cu. ft. of gas from the upper part of the Mississippian limestone. It has opened up a new field and given a further proof of the potentialities of the Southern Plains. The production of petroleum in Canada is shown in Table I. Since most of the yield comes from Alberta, the production is shown from the various fields in Table 2. The sale value of the petroleum produced in Canada in 1940 exceeded 11.1 million dollars, which is still somewhat less than the value of the natural gas production, shown in Table 3. Table i.—Production of Petroleum in Canada" Barrels Province 1939 1940 New Brunswick........ 20,101 21,161 Ontario............... 206,196 186,471 Alberta............... 7,595,000 8,493,237 Northwest Territories. . 17,013 8,493,23717.184 Total............... 7,838,310 8,718,053 Value............... $10,353,351 $11.113,000 0 Bureau of Statistics, Ottawa. Turner Valley, Alberta Turner Valley continues to be by far the largest producing field in Canada (details are given in Table 4), The limits of the Pr in- field are now Known. On the east the oil area is bounded by the gas cap, which in turn is cut off on its east side by a major overthrust fault; on the west, ii is defined by edge water at a level of 4roc

Jan 1, 1941

By G. S. Hume

Production of petroleum and natural .gas increased in Canada in 1940 over the previous year. Alberta produced more than 97 per cent of the total Canadian production of 8,718,053 bbl. of oil, an increase for this province of nearly 12 per cent, whereas in Ontario and New Brunswick, where the production is relatively small, there was a slight decline. In Alberta the main producing field is Turner Valley, on the eastern edge of the foothills southwest of Calgary, and development continued in this field in 1940 with the completion of 36 wells, all of which obtained production. In the Red Coulce field, close to the International Boundary, near Coutts, no new wells were drilled and the seven producing wells showed a decline of 900 bbl. below the previous year. Also, in the Wainwright field of east central Alberta, four wells, yielding heavy crude oil, produced 4000 bbl. less oil than in 1939, owing possibly rather to discontinuous operation than to actual decline in potential yield. This decline was more than offset by production from a new field 40 miles northeast of Wainwright, at Borradaile, producing oil of 14" to I 5° A.P.1. There was a small increase in production during 1940 from the Del Bonita field, in southern Alberta, where the production is from two wells. The outstanding development of the year was the completion of Standard Oil Princess No. 2 well in the Steveville area, on the Plains 100 miles east of Calgary. This well was completed late in December with an initial flow1 of 520 bbl. of 26.3" A.P,I. oil, and 12,750 M cu. ft. of gas from the upper part of the Mississippian limestone. It has opened up a new field and given a further proof of the potentialities of the Southern Plains. The production of petroleum in Canada is shown in Table I. Since most of the yield comes from Alberta, the production is shown from the various fields in Table 2. The sale value of the petroleum produced in Canada in 1940 exceeded 11.1 million dollars, which is still somewhat less than the value of the natural gas production, shown in Table 3. Table i.—Production of Petroleum in Canada" Barrels Province 1939 1940 New Brunswick........ 20,101 21,161 Ontario............... 206,196 186,471 Alberta............... 7,595,000 8,493,237 Northwest Territories. . 17,013 8,493,23717.184 Total............... 7,838,310 8,718,053 Value............... $10,353,351 $11.113,000 0 Bureau of Statistics, Ottawa. Turner Valley, Alberta Turner Valley continues to be by far the largest producing field in Canada (details are given in Table 4), The limits of the Pr in- field are now Known. On the east the oil area is bounded by the gas cap, which in turn is cut off on its east side by a major overthrust fault; on the west, ii is defined by edge water at a level of 4roc

Jan 1, 1941

By J. Chipman, N. J. Grant, R. Rocca

Desulphurization of liquid iron by reducing slags of the electric-furnace type was studied from 65 heats. Variations were made in basicity over a wide range and in FeO up to about 5 pct for their effects on desulphurization. The role of FeO in desulphurization from the blast furnace, to the electric furnace, to the oxidizing conditions of the open hearth is shown to fit a relatively simple pattern of behavior. THE mechanism which controls the desulphurization of molten iron by basic slags has been the object of several investigations. In particular, equilibrium determinations have been made both in the field of basic open-hearth slags, which have a high iron-oxide concentration, and in the field of blast-furnace slags which have a very low iron-oxide concentration. In both cases the desulphurization ratio has been found to increase with increasing basicity of the slags; however, the mechanism of desulphurization differs in the two cases. In basic open-hearth slags desulphurization occurs mainly as a partition of iron sulphide:&apos; FeS * (FeS) and the desulphurization ratio is approximately independent of iron-oxide concentration in the slag. In blast-furnace slags the concentration of iron oxide is very low as a result of the highly reducing conditions in which they are formed. The controlling reaction for desulphurization is then:2,3 FeS + (CaO) <=* (CaS) + (FeO) The slags of the reducing stage in the electric furnace have an iron-oxide concentration which is intermediate between blast-furnace and open-hearth slags. The study of the mechanism of desulphurization for these slags has been the object of this investigation. The importance of low (FeO) in the slag for desulphurization was first verified by Bardenheuer and Geller,& who found that high desulphurization ratios were obtained in highly reduced slags. It was recognized" hat iron oxide in the slag becomes a controlling factor in desulphurization only at FeO concentrations approximately under 5 pct. A recent investigation conducted by Buehl,7 upon the suggestion of one of the authors, confirmed this opinion from the results obtained from a heat conducted in a small arc furnace. In the present investigation, slags of very high basicity, such as often are encountered in the basic electric furnace, could not be studied, but equilibrium data have been obtained for slags in a wide basicity range. The iron-oxide concentration in these slags ranged from 0.08 to 15 pct and was controlled by the addition of silicon to the metal. Other constituents of the slags were mainly CaO, MgO, SiO2, A120,, and CaF,. The experimental technique was essentially the same as that of previous investigations.1 8-lo In an open magnesia-lined induction furnace, 65 lb of Armco ingot iron was melted. An atmosphere of hydrogen was maintained over the melt for 1 hr to bring the carbon content down to approximately 0.010 pct maximum. The bath then was exposed to air for 25 min to remove hydrogen. The electrodes were put in place, and the furnace was operated from this point on in an atmosphere of nitrogen. A synthetic slag was added to which additions of silicon and iron sulphide were made. A rate study conducted at the beginning of this investigation had

Jan 1, 1952

By C. A. Stetefeldt

It will be of interest to compare the statistics of the gas-producer plant at Aspen, Colorado (recorded by Mr. W. S. Morse in a paper read at the Montreal Meeting, February, 1893*), with those at the Marsac mill, Park City, Utah, where such a plant was first introduced by the writer in July, 1890. In both mills a Stetefeldt furnace is used for roasting; but the Marsac mill has the old-fidsdshioned revolving dryers, while at Aspen, shelf-dryers are at hand. At Aspen, separate Taylor-producers are provided for the Stetefeldt furnace and the shelf-dryers; at the Marsac mill one 7-foot producer supplies gas to both the furnace and the dryers. Hence, in the latter case, the quantity of coal consumed for each apparatus can only be estimated, based upon the relative consumption of wood before gas was introduced. According to Mr. Wilson&apos;s statement, the relative consumption of wood in the Stetefeldt furnace and the revolving dryers was as 3 to 2. In the year 1892 the Marsac mill put through the dryers and the Stetefeldt furnace the following quantities of ore and salt (approximate dry weights) : ore, 22,800 tons; salt, 2262 tons. There were consumed in the Taylor-producer 2,714 tons of Rock Springs coal. We may thus make the comparative estimate as follows: Table Showing the Consumption of Coal per Ton Of Ore and Salt at the Marsac and Aspen Mills. Marsac. Aspen. Difference. Pounds. Pounds. Pounds. Drying ore and salt,.... 86.63 72.22 14.41 Roasting ore,.....142.40 117.44 24.96 Total,.....229.03 189.66 39.37 In making a just comparison a number of items must be taken

Jan 1, 1894

By R. W. Carpenter, J. C. Ogle

It is possible, by using pack-rolling instead of conventional rolling, to reduce a number of metals to thicknesses of 2µm or less. Such thinfoils are generally made at room temperature without intermediate annealing. In addition, pack-rolled foils fail by developing pinholes at thicknesses near 2µm instead of developing the shear cracks usually observed in cold-rolled ductile metals. This paper presents the results of a general investigation of the deformation substructure and texture developed in copper and iron pack -rolled from 130 to about 2µm thickness. Electron microscopy showed that in both metals a fine (0.2 to 0.5?µ m) deformation subgrain structure formed during pack-rolling; in neither case was this substructure grossly different from substructures formed during conventional rolling. The deformation texture formed in pack-rolled iron was quite similar to usual bcc textures; however, in the case of copper, the cube texture was stable during pack-rolling and the normal copper deformation texture was unstable. It is shown analytically that the constraining pack induced a large hydrostatic pressure in the foils during pack-rolling. The pinhole failure mechanism is attributed to the presence of the large hydrostatic pressure during pack-rolling; this strongly suppressed the growth of shear cracks. The stability of the cube texture in copper is also probably due to the unusuul stress distribution developed during pack-rolling. EXPERIMENTS at several laboratories have shown that very thin foils of the common structural metals and many of the rare earths can be made by "pack-rolling". 1-3 The technique was originally developed to make specimens for nuclear scattering experiments and foils for X-ray filters. It is also useful for making experimental laminar metallic composite bodies and foils thin enough for direct examination by ultra-high voltage electron microscopy without the need for special thinning techniques. Pack-rolling in the present context means a three-layer pack, with the material to be rolled into foil comprising the center layer. The outer two layers, which constrain the foil during reduction, are ordinarily austenitic stainless steel. Typically, a 130 µm (0.005 in.) metal strip can be reduced to a final thickness of 2 µm or less by this process. This is accomplished at room temperature, without intermediate annealing. It has been observed that foils produced by this process do not exhibit at any stage of their reduction the severe work-hardening found in strip rolled by conventional cold-rolling methods. Neither is the failure characteristic the same."&apos; Conventionally cold-rolled ductile metal strip fails by developing shear cracks on planes whose normals nearly bisect the angle between the rolling direction and normal to the rolling plane; these are planes of maximum shear stress. In pack-rolling this mechanism has not been observed; failure occurs by the formation of pinholes on the foil surface (penetrating the foil). If pack-rolling is continued the hole density increases. These differences in behavior imply the existence of appreciably different substructure in pack-rolled foils compared to substructure in conventionally rolled material, or perhaps that the geometry of pack-rolling has an effect on the foil behavior. This paper describes an investigation of deformation substructure and texture in some specimens of pack-rolled copper and iron, and some considerations of the stress distribution in the foils during rolling that result from the geometry of pack-rolling. EXPERIMENTAL DETAILS Three different materials were used for pack-rolling in the present work: soft copper sheet (99.8 pct Cu, 0.03 pct 0, electrolytic tough pitch) and two types of iron, Ferrovac E* and Armco iron. Each was "Crucible Stccl Co. initially in the form of 130 µm annealed strip with grain size ranges of approximately 10 to 40 µm. The initial texture of the copper (determined as noted below) was the normally observed cube type (001)[100]; there was evidence of a small amount of material in the cube-twin orientation reported by Beck and Hu.4 The initial texture of the Ferrovac E was similar to that reported for recrystallized iron by Kurdjumov and sachs,5 who list the principal orientations as {111}<112>, {001}<110> 15degfrom RD and a weak component {112}(110) 15 deg from RD. The starting texture of the Armco iron was not determined. Pack-Rolling Procedure. A four-high mill was used for all specimens. The work roll and backing roll diameters were 1.625 and 5.25 in., respectively. The peripheral roll speed of the work rolls was about 2.5 in. per sec. All foils were initially reduced from 130 to 100 µm by conventional straight rolling and then inserted into a pack, without any intermediate annealing, for further reduction. The pack consisted of an 0.033 in. (838 µm) thick 3 by 6 in. polished sheet of austenitic stainless steel, folded to make a 3 by 3 in. jacket. After folding, the jacket was given a small reduction to close the fold tightly before insertion of the foil. During pack-rolling a constant change in roll spacing was made every third pass. The roll-spacing change corresponded to a 5 pct reduction in thickness for a new pack. This approached a 10 pct reduction when the pack had decreased to about half its original thickness. At this point the deformed pack was discarded and a new one

Jan 1, 1970

By W. N. Miner, R. O. Elliott

Electrical-resistivity )measurments were made be-trueetz room temperatrive and 1.5 oK on five different stocks of cerium metal, and the results were correlated with the types, amounts, and distribution of the impurities present. Magnesium, which appeared to be distributed as a solute throughout the cerium matrix, was found to have a large effect on the residual resistivity, 1 at. pct Mg being sufficient to increase the residual resistivity by about 10 microhm-cm. The formation of ß by repeated thermal cycling between room temperature and liquid-helium temperature is attributed to the deformation and faulting that occurs during the ? D a transformation. In preparation for starting a proposed study of cerium-rich alloys, we examined samples from severa1 stocks of cerium metal in order to choose the purest stock for future use in making the alloys. Low-temperature electrical-resistivity data were used to gain initial information about the purities of the stocks. Additional information was subsequently obtained from chemical analyses, density measurements, optical metallography, and electron-micro-probe analyses. Cerium that has been annealed at high temperature and cooled to room temperature has the fee crystal structure (? phase) with a = 5.16Å. When cooled further, in the region between about 250" and 150°K, some of the fee phase transforms to the double hcp form (ß phase) with a = 3.68 and c = 11.92Å. The remainder of the room-temperature fee form (and perhaps some of the hexagonal phase) transforms electronically in the vicinity of 100° K to the more dense or "collapsed" fee form (a phase), a - 4.85A, by transferring about 0.5 electron per atom from the 4f level to the valence band. Very little work related specifically to the effects of impurities on the physical properties of cerium has been reported in the literature. Gaume-Mahn1, 2 has studied the effects of calcium, magnesium. iron, silicon, and tantalum on the electrical resistivity and magnetic susceptibility of cerium between 60o and 300°K. Gschneidner, Elliott, and McDonald3 have discussed the effects of total impurity content on the hysteresis of the a —? (reversible) transformation and on the formation of the 4 and "a-? intermediate" phases. Smith and Morrice* have reported the effect of total impurity content on the resistivity of cerium at 4 and 293°K. In none of these reports, however, is it apparent that the distributions of the impurities were determined, L.r., whether the impurities were present in inclusions or in solid solution in the matrix is not mentioned; nor does it appear that the phase purity of the cerium was always considered. In the present study, five different stocks of cerium were involved. One was represented by a single sample of electrowon cerium, which was all that had remained from a stock of high-purity material obtained from the U.S. Bureau of Mines, Reno, Nev., in 1959. The other four stocks were recently purchased from commercial sources and were specified to be 99.9 wt pct pure. EXPERIMENTAL Cerium stocks designated as #1, #2, #4, and #5 were obtained from commercial suppliers for the specific purpose of finding a reliable source of high-purity cerium. Although the purity level of the cerium was specified to be 99.9 pet, the specifications did not include limits as to the amounts of various impurities that would be acceptable. Consequently the chemical analyses of the different stocks varied widely. Stock #3, which had been obtained from the U.S. Bureau of Mines and which was the purest on the basis of chemical analyses, consisted of a single specimen of electrowon cerium. It was included in the examination for purposes of comparison. Table I contains the chemical and spectrographic-

Jan 1, 1968

By T. E. Evans, C. T. Baroch

ZrB2 was produced in batches of 4 to 6 Ib by interaction of ZrO2, B4C, B203, and carbon at around 2000°C in a simple graphite resistance furnace. Techniques of production are discussed and the final design of a suitable furnace is described in detail. Several other borides were made by the same technique and the process appears to have possibilities for commercial production. N seeking out new hard and refractory com- pounds, many researchers have turned to the investigation of the borides and excellent papers have been published on the properties of these compounds. Few papers, however, have appeared on the techniques and problems concerned with the production of these high temperature substances. This report describes progress made in developing a method for preparing zirconium diboride, ZrB2, on a pilot plant scale. The literature of the borides and other refractory hard metals recently has been reviewed, annotated, and classified so completely&apos; that it is needless to attempt such an outline here. It is enough to say that three borides of zirconium have been reported: ZrB, ZrB2, and ZrB12.2 ZrB2 is the most stable of these and is especially stable in the presence of carbon up to and including its melting point of around 3000°C. Like most borides, it can be prepared in several ways. It can be prepared by synthesis of the elements, but these are expensive and difficult to produce in a high state of purity. Obviously, production directly from the oxides would have decided economic advantages. In electrolytic production such as that of calcium boride,:&apos; the product is recovered as a sludge mixed with electrolyte; and separation of product from adhering electrolyte and regeneration of the electrolyte is an involved and difficult process. The work on borides was started on a small scale in 1948. Late in 1949, Naval Ordnance expressed a specific interest in ZrB2 and the project then centered on this compound. After the usual experimental work necessary in a new field, ZrB2 of good quality was produced by heating mixtures of B4C, ZrO2, B2O3, and carbon to a temperature of about 2000 °C in a resistance-type electric furnace. Over 100 lb was made for experimental use tests, and the method of production probably could be expanded into a commercial operation. A similar process has been described by Kieffer and coworkers.&apos; The main chemical problems were the development of proper charges to insure complete reduction of the elements, determination of the proper temperature range at which these reductions took place, and adoption of techniques necessary to pre- vent inclusion of such impurities as carbon and nitrides. The mechanical problems consisted of developing a simple practical furnace that would attain the high temperatures required and permit use of a controlled atmosphere when necessary and determining of suitable refractories. Both problems were solved by designing a crucible resistance furnace. Crucible Resistance Electric Furnace Attempts were first made to produce ZrB2 in an electric arc furnace, but such a furnace would not provide the degree of carbon control required for producing clean graphite-free borides, so it was decided to try working in a crucible. Obviously, the furnace would have to be constructed of graphite, as the temperatures required are too high for other refractories or heating elements. Crucibles were made by hollowing out segments of graphite electrodes, which were fitted with a cover and clamped between two electrodes so that the current passing through the thin wall of the crucible would generate heat, using the principle of the Helberger crucible furnace."? Preliminary tests with this type of furnace were encouraging and led to the furnace design shown in Fig. 1. The essential components were a thin-walled graphite crucible resting on a graphite block, which formed the lower electrode assembly, and a top electrode assembly swung from a pipe column making contact with the top of the crucible. The space around the crucible was filled with graphite prepared from waste electrodes crushed to about ¼ in. This packing had excellent insulating properties, both electrically and thermally, and could be removed easily and quickly from around the crucible by means of an industrial vacuum cleaner. The largest resistor crucibles were machined from 8 in. electrode stock and were 26 in. long, with a side wall Yi in. thick and a 1 in. bottom. Temperatures were determined optically by sighting down a 1 in. hole drilled longitudinally through the top electrode and the crucible cover. Sealing this hole at the top was a water-cooled brass sight-glass assembly, shown in Fig. 2. An opening was provided for a light flow of helium to keep the sight opening clear of smoke, and a glass prism above the sight glass changed the line of sight to the horizontal for easier reading. More recently, the prism and optical pyrometer were replaced by a photoelectric recording pyrometer. At first the charges were placed directly in the resistor crucible but this meant that everything had to be withdrawn from the furnace every time the charge was emptied. Later, smaller crucibles were made up that could be placed inside the resistor

Jan 1, 1956

By W. A. Tiller, W. C. Johnston

The solute distribution ahead of an advancing solid-liquid interface is controlled by varying the momentum boundary layer thickness in the liquid adjacent to the interface. Single pass zone-melting experiments on Pb-Sn alloys are described in which the liquid is caused to rotate in the plane of the solid-liquid interface due to the influence of a magnetic .field rotating in this plane. The variation of the diffusion boundary layer thickness with field strength is determined. DURING the freezing of an alloy a partitioning of solute occurs at the solid-liquid interface, the magnitude depending upon the difference in the solid and liquid solubilities at the interface temperature. Because the diffusion coefficient is so small in the liquid relative to normal freezing rates, either a pileup or a depletion of solute occurs at the interface when the partition coefficient, kO, is either less than or greater than unity, respectively. This solute distribution is completely characterized by i) the solute concentration in the liquid far from the interface, C) the ratio of freezing velocityf, to diffusion coefficient, D, iii) the partition coefficient, ko, and iv) the thickness of the diffusion boundary layer, 6,, at the interface (this assumes that an electric field is not applied across the interface). For a particular system, C ko and D are fixed so that the character of the solute distribution can be changed only by a variation of either f or 6c. As is well known, the freezing velocity can be changed by varying the thermal environment of the alloy. Whereas, the thickness of the solute rich layer can be changed by varying the fluid flow conditions in the liquid. It is the purpose of this paper to describe a technique for controlling the fluid flow conditions in the liquid. During most solidification experiments the driving force for fluid flow arises from either mechanical mixing, thermal convection or electromagnetic mixing. The momentum boundary layer thickness, 6m at the solid-liquid interface, within which negligible movement of the liquid occurs, has been calculated for the special case of mechanical mixing where crystals are solidified by the Czochralski technique.l,2 The calculation of 6m for the case of thermal convection has also been made.3 In some calculations it has been assumed that the momentum boundary layer thickness, 6,, may be equated to the thickness of the diffusion boundary layer 6c, at the interface. However, as may be seen from Appendix I this is only true in very special cases and in general where a is a constant of magnitude determined by the particular liquid alloy. Neither calculations nor experimental data exist for the dependence of upon electromagnetic mixing. In this paper experiments are described in which the liquid is caused to rotate in the plane of the interface due to the torque developed on it by a magnetic field, H, rotating in this plane. The variation of is controlled by the variation of H. A magnetic field rotating in a plane perpendicular to the interface has been used for the purification of aluminum. Experimentally, we determined the variation of 5C with H by using the zone-melting technique of pfann5and a theoretical relationship of Burton et a1.2 pfann5 has shown that, after the passage of one molten zone through a long cylindrical charge of uniform concentration, CO, the solute distribution, C,, in the solid is as shown in Fig. 1. The equation describing this distribution is

Jan 1, 1962

THE papers by G. F. Loughlin and I. A. Ettlinger discussed the distribution of formations and ore-bodies in two of the main mining districts of the Southwest. The convergence of the deeper orebodies at Cripple Creek points to their common hypogene ori-gin, as do the occurrences of the copper ores of, central Arizona. E. L. Bruce described the areas in southwestern On-tario around Red Lake and Woman Lake, another prom-ising gold district. Of special interest was a series of lantern slides showing the use of power-driven boats and of hydroplanes as means of transportation. Within a few years, no doubt; such devices will revolutionize the mining industry and reconnaissance mapping in these relatively inaccessible areas. Much interest was evinced in the paper by J. W. Finch on "Sedimentary Metalliferous Deposits of the Red Beds." It was written as a caution to people at-tempting to mine these deposits. The discussion of the chemical equations presented in the paper brought out the fact that a large amount of study of such ores is necessary before we shall be able to write equations to explain their formation. Especially pertinent were the discussions by David White as to the relation of decay-ing plant tissue to metalliferous deposits and the color of sediments; also the point brought out by T. S. Lover-ing that chemical compounds produced by bacteria may greatly affect the deposition and reorganization of sedi-mentary metalliferous deposits.

Jan 3, 1928

By Klaus Schwerdtfeger

The rules of solution of oxygen from H2O-H2-He gas and of nitrogen from N2-H2 gas in shallow melts of liquid iron were measured at 1610o and 1600o C, respectiuely. Concentration profiles were detemined in the liquid iron. Tire rate data indicate that the solution process is controlled by diffusion in the iron melt. The diffusivities for oxygen and nitrogen in liquid iron, as calculated from the present data, are DFe-o = (12 ± 3) < 10-5 sq cm per sec and DFe-N = 11 ± 2) X 10-5 sq cm per sec at the temperatures employed. AN attempt was made by Shurygin and Kryukl to measure the diffusivity of oxygen in liquid iron. In their experiments a silica disc was rotated in liquid iron containing oxygen, and the rate of formation of liquid iron silicate was measured. Assuming that the rate of dissolution of silica is controlled by diffusion of oxygen in the iron, the oxygen diffusivity was computed from the rate data giving Dfe-0 = 6.1 X 5 sq cm per sec at 1600°C. Although this value seems to be of the right order of magnitude, there is no proof of the correctness of the assumptions involved in the interpretation of these rate data. The oxygen concentration in the iron at the iron-iron silicate interface was taken to be that in equilibrium with the silica-saturated silicate melt. That is, it was assumed that no concentration gradient existed in the liquid silicate. This is a questionable assumption, unless it is proved that the thickness of the silicate layer is very much smaller than that of the diffusion boundary layer in the iron. Furthermore, Shurygin et al.1 used the Levich equation2 to interpret their rate data. This equation was derived for mass transfer between a solid disc and a single-phase liquid. The hydrodynamic and diffusion boundary layers in the iron stirred by a disc, via coupling of the silicate melt, may be appreciably different from those predicted by Levich&apos;s derivations. In the present work the diffusivities of oxygen and nitrogen in liquid iron were measured at 1610" and 1600oC, respectively. EXPERIMENTAL METHOD Iron melts contained in high-purity gas-tight alumina crucibles were reacted with H2O-H2-He gas for the determination of the oxygen diffusivity and with N2-H2 gas for the determination of nitrogen diffusivity. At the end of the reaction period, the samples were quenched in a cold H2-He gas stream at the top of the furnace. Oxygen or nitrogen contents in the iron were determined by chemical analysis. Two different types of diffusion experiments were perforxed. To determine concentration profiles, a few rate measurements were made using 4-cm-deep melts. The solidified samples were sliced into discs and each disc was analyzed for oxygen or nitrogen. In another series of experiments, oxygen or nitrogen was diffused into shallow melts (about 0.5 to 1 cm in depth) and the total sample was analyzed to obtain an average concentration of the diffusate. In most experiments, 4- to 5-mm-ID alumina crucibles were used. Some experiments were also made in smaller (3 mm) and larger (7 mm) diam crucibles. This variation in diameter caused no difference in the reaction rate, within the limits of experimental uncertainty. To promote the establishment of a stable density profile in the melt, all the samples were suspended in the lower end of the hot zone so that the top of the melt was hotter by a few degrees. Molybdenum wire resistance heating was used. The reaction tube of the furnace was a gas-tight recrystal-lized alumina tube. In most experiments the furnace was heated by an ac power supply. To check the possibility of inductive stirring, some experiments were carried out in a dc operated furnace, with essentially the same results. The temperature of the furnace was controlled automatically in the usual manner. The temperature was measured with a Pt/Pt-10 pet Rh thermocouple and is estimated to be accurate within ±5°C. The iron used was prepared by melting and vacuum-carbon deoxidizing electrolytic "Plastiron" in a zir-conia crucible. The main impurities are: Si 0.004 pct P, S <0.002 pct Cr 0.005 pct N 0.001 pct Zr 0.002 pct O 0.003 pct Mn 0.004 pct C 0.002 pct The gas composition was controlled by constant pressure head capillary flowmeters. Oxygen was removed from the gas mixture by passing it through columns of platinized asbestos (450°C) and anhydrone. Selected H2O contents were obtained by passing the purified gas through oxalic acid dihydrate-anhydrous oxalic acid mixtures held at constant temperature in a water bath. Water vapor pressure data for the oxalic acid dihydrate-anhydrous oxalic acid equilibrium were taken from the 1iterature.3 The flow rate used was about 1.5 liters per min. The whole system was checked for tightness at regular intervals.

Jan 1, 1968

By E. D. Gardner

Apparently the widespread agitation for the codification of our mining laws has had its effect, and it is quite possible that Congress will take up the question during this present session. The greatest objection to our present statutes pertaining to metalliferous deposits seems to be directed against the law of the apex. Those who are not in favor of changing this law are very far in the minority and they apparently realize that it is useless to urge its retention. Next in importance to the repeal of the law of the apex, seems to be a widespread advocacy for the repeal of the law requiring discovery of mineral before a valid location of a mining claim can be made. To a lesser extent there appears to be a desire to have the law changed so as to allow patent for claims without mineral discoveries. The purpose of this article is to review the arguments in favor of the proposed change of the discovery requirement, to show some of the evils that may be expected to result therefrom, and to consider whether a system may be devised to correct the undesirable features of the present law in this respect and at the same time not expose the mining fraternity and the general public to the evils which would result from the repeal of this fundamental requirement. Under the law as at present framed, the validity of a mining location is dependent upon the fact of discovery of mineral within the boundaries of the land claimed. " * * * but no location of a mining claim shall be made until the discovery of the vein or lode within the limits of the claim located" (Sec. 2,320, U. S. Rev. Stat.). All authorities agree that discovery is the source of the miners&apos; title. Lindley, in his valuable work on Mines (3d Ed., Sec. 335), lays down the rule in part as follows: "Discovery is the initial fact. Without that no right can be acquired. * * * Such discovery must precede the location, or be in advance of intervening rights. The proof of recording and marking a claim will not authorize the court to presume a discovery." As is well stated by the U. S. Supreme Court in Erhard v. Boaro (113 U.S. 536):

Jan 1, 1917

By F. W. Aul, R. C. Glenn

EXTRACTION techniques are of particular importance in determining size, shape an: crystal structure of particles smaller than l000Å in steels and other alloys. However, artifacts that can arise during the preparation of extraction replicas may lead to erroneous conclusions. The purpose of this note is to illustrate some of these artifacts and the misinformation that can result from their presence. An alloy of iron with 0.8 pct Cu was investigated in the following conditions: 1) Solution treated 3 days at 925°C in dry hydrogen and quenched in water. Aged in steps to precipitate copper, as follows: heated to 700°C, held 1 day; then furnace cooled to 50O°C, held 3 days; then furnace cooled to room temperature. 2) Solution treated 3 days at 925OC in dry hydrogen and furnace cooled to room temperature. 3) Solution treated 3 days at 925OC or 17 hr at 1100°C in dry hydrogen to dissolve all copper, then quenched in water. A normal parlodion dry-extraction technique was employed after etching the specimens with super picralP or with 2 pct nital. A wet-extraction method

Jan 1, 1962

By C. C. Harris

The 3-parameter equation* was introduced1 as having the necessary form and flexibility for describing the major features of size distribution curves. Also, Eq. 1 was shown to contain most of the widely used 2-parameter equations as special cases. Special methods are necessary in order to determine the parameters of 3-parameter equations by graphical means. The procedure given previously required double graphical interpolation followed by regraphing the interpolated data. The theoretical basis of the method was a difference equation eliminating y. Several other methods for obtaining the parameters have been under development and one method appears to overcome the disadvantages of the earlier method and satisfies several procedural requirements. The points in favor of the new method as compared to the earlier method are as follows: 1. Estimation of the quality of fit is direct, and is in fact an essential part of the procedure. 2. The data is plotted directly without the necessity of interpolation from a graph. 3. The method makes use of Rosin-Rammler2 paper which because of expanded scaling in the coarse sizes leads to improved accuracy1 as compared with the log-log plot for the Gates3-Gaudin4-Schubann5 representation. 4. There is a gain over the earlier method in overall accuracy and in simplicity.

Jan 1, 1970

By F. von Gemmingen, E. J. Fasiska, L. Zwell

EARLIER studies of the dependence of creep on structure1 and of the dependence of creep rupture on creep behavior2 did not include detailed discussion of the phases present in the specimens under examination. It is of interest to determine the nature and amounts of such phases present since it is well known that these are dependent on composition, heat treatment and creep conditions.3 This investigation has therefore been undertaken to identify these constituents and to determine their relative amounts. This report presents the results of this investigation and describes an improved "extraction replica" technique developed in the course of the work. The composition of the Type 316 austenitic stainless steels studied in this investigation is given in Table I. The specimens were solution treated at 2000°F for 1/2 hr and water quenched. Those specimens subjected to prestrain at room temperature Methods for extracting precipitate particles from materials for electron and X-ray diffraction analysis have been described by Fisher,4 Smith and Nutting: and Booker and coworkers.6&apos;7 Electrolytic extraction methods have been described by Andrews and Hughes.8 The first two methods have been used at this Laboratory, but have not proved satisfactory for many problems requiring X-ray diffraction analysis. It has been difficult to remove the replicas or to avoid tearing them during removal. These difficulties are overcome by backing the replica with a water-soluble plastic such as Dupont 51-05 Elvanol (polyvinyl alcohol). The backing increases the thickness of the replica so that it can be mechanically stripped from unloosened particles without folding or tearing. This procedure eliminates the stripping of wet replicas, which usually have a low tear strength. By stripping replicas after drying, it is possible to extract partially loosened particles which otherwise would remain imbedded in the metal. The modified method is as follows: after the specimen is polished, it is etched for 60 min in modified glyceregia consisting of 30 ml glycerol, 7 ml nitric acid, and 4 ml of hydrochloric acid. The sample is then washed, air dried, and coated with a 20 pct Baker and Adamson 1611 collodion (85 pct amyl acetate by volume) film. After the collodion film is dry (about 15 min), the sample is again etched in the modified glyceregia for 50 min, washed with isopropyl alcohol (to prevent dissolving the collodion) and air dried. A very thick coat of polyvinyl alcohol (about 50 pct solution "Elvanol Dupont 51-05" in water) is poured over the sample and is permitted to dry for about 24 hr. The composite film containing the precipitates is then stripped from the specimen and floated, polyvinyl alcohol side down, in water (at about 50°C) until the polyvinyl alcohol dissolves. This usually takes about 15 min. Should any of the polyvinyl alcohol remain on the replica, it does not give a crystalline diffraction pattern and therefore does not hinder identification of the precipitates. The extraction replica, floating in water, is picked up on a glass fiber and mounted in the Debye-Scherrer camera for X-ray diffraction analysis. Concentration of the etchant, and also etching time, had to be increased for several of the samples. Fig. 1 shows two extraction replicas taken from different areas of spec. M74-37; X-ray analysis showed a strong diffraction pattern of M23C6 and a medium one of u phase. A

Jan 1, 1962

By M. Bevis, A. G. Crocker

A. G. Crocker and M. Bevis (Battersea College of Technology)— Richman and Richman and conard17 have recently published the very interesting results of their studies on the plastic deformation of Fe-Ni-C martensites and of an Fe-5 wt pct Be alloy. Other work on the range of Fe-Be alloys containing between 16 and 27 at. pct Be has also been reported by Richman." One of the fascinating features of this work is that the materials investigated deform primarily by means of twinning and that several twinning modes are operative in addition to the well-established (112 ) mode of bcc materials The composition planes of these unusual twins were determined using a single-surface analysis and reported as (0131, "{045)" or "{089)", and "{2,3,10)" or "(127)". (It is now thought1&apos; that the "{0,1,13)" habit reported for the Fe-Ni-C alloys&apos;&apos; is more likely to be near "{127)". Although the full twinning elements of these unusual twinning modes could not be determined directly from the experimental results, the authors attempt to deduce the elements by considering twin intersectionslQ and by using the projection technique of Jaswon and Dove.&apos; The basic assumption of their approach is that the (013) habits are truly rational planes but that the other habits are irrational and merely approximated to by the indices quoted above. They thus deduce that the twinning mode describing the (013) habit is either Type I or compound and that the modes describing the other habits are Type 11. This deduction must however be false as all twinning modes in cubic structures obeying the classical orientation relationships of deformation twinning must be compound. Type-I and Type-I1 modes can occur in all of the other crystal systems (indeed in the triclinic system compound modes are not allowed), but in the cubic system only compound modes can arise. This fact, which does not appear to be well-known, fol- lows immediately from the relations between the four twinning elements defining a twinning mode. Thus for a Type-I mode which is uniquely defined by the rational twinning elements K1 = hi and tj2 = vi (i = 1, 2, 3), the Kz qd 771 elements are given by: where the summation convention of the tensor calculus has been adopted. For cubic materials the metrics cij Iand cij reduce to the unit tensors 6ij and 6ij so that we have It is clear from these equations that both ki and ui must take on integral values; i.e., Kz, and ql must be rational, if hi and vi are integers, i.e., if K1 and 77~ are rational. Thus for cubic materials a Type-I mode must degenerate into a compound mode and the same result also arises for Type-II modes. The apparently irrational habits observed by the authors can thus not be explained in terms of Type-I1 twinning if the classical laws of deformation twinning are to be obeyed. An alternative explanation of the irrational habits is that they may arise from twinning modes with four irrational twinning elements. These modes, which do not obey the classical orientation relationships associated with deformation twinning, have been shown to arise as the result of double twinning processes in magnesium,22 but may also describe a simple shear on an irrational plane in an irrational direction. Indeed double twinning processes in bcc

Jan 1, 1963