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Jan 1, 1985

By R. H. Marshall, J. Welchner, E. S. Rowland

THIS paper presents results on an exten¬sion into the realm of high-carbon steels of some work recently published' on the effects -of time at temperature, quenching temperature and prior structure on the hardenability of one 0.20 and four 0.40 per cent carbon alloy steels. It was shown at that time that unless the conditions of time, temperature and prior structure are substantially the same in performing the hardenability test as in conducting harden¬ing of parts in production, the correlation of hardenability information with the [ ] hardness and properties of production parts is often not of satisfactory accuracy. The general effects of these variables on the austenitic grain size, distribution of excess carbides and critical cooling rate have been known for many years and one or more have been investigated by Shepherd ,2 3 Davenport and Bain,4 Digges,5,6 Digges and Jordan,7 Post and associates' and Roberts and Mehl,9 to mention only a few. There has been no systematic investigation, however,' into the quantitative variations produced on the hardenability of commercial high¬carbon steels by changes in these factors of time, temperature and prior structure. PROCEDURE A plain carbon hypereutectoid steel, S.A.E. 52100 and Graph-Mo, a molyb¬denum-bearing high-carbon steel contain¬ing some graphite, were chosen for this investigation. The chemical analyses of these electric-furnace steels are given in Table I. [ ] The procedure used was exactly that reported previously,' hence the details will not be repeated here. Normalized (1650°F.) and spheroidized prior structures were utilized on all steels with hot-rolled and quenched (1600°F. oil) prior conditions added for the plain carbon steel. The end-quench test developed by Jominy10 was selected for use in this investigation and, with the noted exceptions, the American Society for Testing Materials standard. procedure was followed. The effect of time at temperature was examined at intervals of 0, 10 and 40 min. and 4 hr., and a few i6-hr. tests were run. Salt-bath heating of the specimens was employed to control and minimize the

Jan 1, 1944

By L. W. Reynolds, R. F. Campbell, K. G. Carroll, S. H. Ballard

Based on metallographic and X-ray data probable equilibrium conditions from 1340" to 2400°F are presented for the composition range investigated. These are correlated with investigations of Takei and Kuo. Provision is made for existence of Mo, C and (Fe, Mo)2,C, carbides heretofore omitted in diagrams in this composition range. These carbides and (Fe, Mo),C, in equilibrium with ferrite and austenite, restrict the austenite and austenite + ferrite fields to lower carbon contents and higher temperatures than in the Fe-C system. OK groups of steel of different molybdenum content, but with approximately the same carbon variation in each group, Table I, were studied. The alloys were melted in an acid-lined 30-lb high-frequency induction furnace, and the ingots forged to l-in. rounds, which were then ground to 0.75-in. diam. To minimize chemical segregations a short length of each bar was given a high-temperature heat treatment as listed in Table I. Specimens 0.062 to 0.125-in. thick were thereafter cut from the homogenized bars for heat treatment to determine phase changes in the alloy. Heat treatments were performed in either a lead bath or muffle-type electric furnace, depending upon the temperature required. Maximum temperature variation was * 2" F in the lead bath and * 5"F up to 1900°F and +8"F above 1900°F in the electric furnace. Adequate protection of the specimen from the oxidizing atmosphere in the electric furnace was obtained by sealing the specimen in either a pyrex or a silica capsule which was evacuated or not as circumstances required. For austenitizing followed by quenching to an isothermal temperature, the specimen was placed in a closed-end refractory tube the mouth of which, extending beyond the furnace, was connected to a vacuum pump. The specimen could be withdrawn from this tube and quenched as desired. IDENTIFICATION OF PHASES The principal method of identification of phases was metallographic examination conducted on surfaces well removed from exposure to lead or atmosphere effects during heat treatment. Hardness measurements (Dph/lOkg) were also made on these surfaces. The etching reagents used and their effects are listed in Table II. Martensite and ferrite were readily recognized by their customary appearance after etching with saturated picral or 1 pct nital. The presence of liquid at high temperature was indicated by curved interfaces characteristic of boundaries between solid and melt, by intergranular pools of dendritic areas in a carbide matrix, and by a black network coincident with austenite grain boundaries. Examples of these structures are shown in Figs. l(a) and (0). The types of carbide which were attacked by the electrolytic chromic acid etch and the alkaline KMnO, etch, Table 11, were identified by X-ray analyses of extracted carbides of five alloys. Carbide residue was obtained from a metallographic specimen by etching the specimen for 24 hr in hydrochloric-picric acid in alcohol (grain-size reagent), after which the carbides, standing in relief, were scraped from the surface of the specimen and mounted on a glass slide. Diffraction patterns were obtained with a Philips spectrometer using iron-filtered cobalt radiation. Figs. 2, 3, 4, and 5 illustrate typical etching behaviors with chromic acid and alkaline KMnO,. Chromic acid attacked Mo,C as shown in Figs. 2(a) and (b)-but not (Fe, Mo),C, Fig. 3(b). Alkaline KMnO, attacked (Fe, Mo),C, Fig. 3(c), and also attacked M0,C. In accordance with these behaviors, a typical differentiation of coexisting Mo,C and (Fe, Mo),~ is shown in Figs. 4(a) and (b). The carbide (Fe, Mo),,C, could not be obtained free of other coexisting carbides for etching experiments. The behavior. however. of coexisting carbides identified by x-ray diffraction as Mo,C ind (Fe, Mo),,C, indicate that (Fe, Mo)23C6 is not etched by chromic

Jan 1, 1961

By L. J. Gurevich

IN the course of the examination, at the Bureau of Standards, of fusible tin boiler plugs for the Steamboat Inspection Service, it became evident that an investigation should be undertaken to determine the precautions necessary in the manufacture of acceptable plugs. The results of the tests of these plugs show that their manufacture has improved, though at present not all of the plugs tested are satisfactory. Table 1 gives the result of tests of some 1500 plugs from about 100 makers. Records of the tests show that several of the makers were able to produce satisfactory plugs with every pouring. The Steamboat Inspection Service has the following specifications for fusible plugs: "Fusible plugs for use in boilers of steam vessels under the Jurisdiction of the Steamboat Inspection Service shall be made of bronze casing with the bore tapering continuously and openly from end to end, and filled from end to end with tin not less than 99.7 per cent. pure and to contain not more than 0.1 per cent. of lead and not more than 0.1 per cent. of zinc. The small end of the bore may be countersunk not more than 1/32 in. in depth and width, but no recess, thread, or cavity other than this countersink shall be allowed."

Jan 8, 1919

By R. F. Miller, R. F. Campbell

Sixteen steels containing different combinations of chromium and molybdenum, in amounts up to 5 per cent of each element, were examined for microstructure and hardness after air cooling and after furnace cooling from suitable austenitizing temper- atures. Diagrams summarizing the structnres and hadness resulting from these two cooling rates are presented (Figs. 3, 4, 7).t Data were also obtained on the influence of these two elements, individually and in combination, on the depth of decarburiza-tion observed after furnace cooling (Fig. 8). Composition of Material The chemical composition of the steels investigated is given in Table I. The plain carbon steel was made in a 2 5-ton Heroult electric-are furnace, while the alloy steels were made in a 4.5-ton Ajax-Northrup elec- tric induction furnace. The cast ingots were hot-rolled to 1.75-in. bars. Air-cooled Series The I.75-in. bars were forged to flat plates, 0.25 in. thick, from which specimens 0.5 in. wide by 2 in. long were cut. The specimens were pretreated to improve their homogeneity by heating to 1830°F. (I000°C.) for 20 min. and oil-quenching. They were then reheated to 1740°F. (950°C.) for one hour and air-cooled, after

Jan 1, 1942

By R. F. Campbell, R. F. Miller

Sixteen steels containing different combinations of chromium and molybdenum, in amounts up to 5 per cent of each element, were examined for microstructure and hardness after air cooling and after furnace cooling from suitable austenitizing temper- atures. Diagrams summarizing the structnres and hadness resulting from these two cooling rates are presented (Figs. 3, 4, 7).t Data were also obtained on the influence of these two elements, individually and in combination, on the depth of decarburiza-tion observed after furnace cooling (Fig. 8). Composition of Material The chemical composition of the steels investigated is given in Table I. The plain carbon steel was made in a 2 5-ton Heroult electric-are furnace, while the alloy steels were made in a 4.5-ton Ajax-Northrup elec- tric induction furnace. The cast ingots were hot-rolled to 1.75-in. bars. Air-cooled Series The I.75-in. bars were forged to flat plates, 0.25 in. thick, from which specimens 0.5 in. wide by 2 in. long were cut. The specimens were pretreated to improve their homogeneity by heating to 1830°F. (I000°C.) for 20 min. and oil-quenching. They were then reheated to 1740°F. (950°C.) for one hour and air-cooled, after

Jan 1, 1942

By H. F. Webster, C. G. Dunn

Rolling md annealing procedures are described for developing the (110) preferred orientation in tantalum for use as a thermionic-emission materinl where electrodes of a uniform high work function are needed. The development of a (110) [001] annealing texture is also reported. A preferential growth process due to low (110) gas-metal surface energy is considered in explanation of the observed growth of (110) grains. ThE growth of (110)-oriented grains in thin strips of rolled zone-refined tantalum, previously discussed briefly,' is reported together with more recent information on the formation of a (110)[001.] annealing texture, i.e., one where the [001] direction of each grain lies close to the rolling direction. The development of tantalum sheet with a (110) preferred orientation (position of [001 ] directions unspecified) is of importance as a thermionic-emission material in thermionic-energy converters. Since therm ionic-emission properties of cesium-coated crystals vary over a wide range depending on (hkl) a2-7 a single (hkl) preferred orientation is more useful than either several preferred orientations or none. Furthermore, the (110) preferred orientation yields the highest thermionic-emission density for a cesium coverage of less than a monolayer.5-7 A consideration of the stability of the grain structure needed at high operating temperatures suggests that the preferred orientation itself should be produced by annealing processes. Information on annealing textures in tantalum, however, is rather limited. Pugh and Hibbard 8 obtained (111)[112] and (lll)[112] components in a 1400°C recrystallization texture in 95 pct cold-rolled foil; these components were enhanced on annealing at 2500°C. Muller9 rolled 99.97 Ta to 90 pct reduction in thickness in the final stage and noted only a slight sharpening of the rolling texture, with some intensification of the (111)[112] component upon annealing at 1200°C. The experimental procedure followed in the present work stemmed from the idea of using possible differences in (hkl) surface energies to provide a small driving force for growth of grains having the lowest (hkl) surface energy.l0* This would mean using high-purity tantalum processed into thin sheet form and annealed at high temperatures either in a noncontaminating atmosphere or in one producing additional sample purification. EXPERIMENTAL Zone-Refined Tantalum. National Research Corp. tantalum in the form of 1/8-in.-diam rod and of 99.98 purity (53 ppm 0, 15 ppm N, and 8 ppm C) was zone-melted four times. The traversing speed was 4 mm per min. Such treatment increased the resistance ratio, R293k/R20K , where R293K is the resistance of the specimen at 20°C and R20K the re-resistance at liquid-hydrogen temperature, from a value of 25 for the initial rod to 175 for the zone-refined rod (the increase in the resistance ratio provides a measure of purification11,12). Part of a zone-refined rod was rolled unidirec-tionally to a strip 0.003 in. thick and 0.28 in. wide. Samples were given anneals in the range 1300" to 2100°C using ac conduction heating in an oil-free vacuum system. Recrystallization to small grains appeared to be complete at 1300°C. Large grains were formed at higher temperatures, but these were not entirely strain-free, some grains showing asterism in Laue X-ray patterns and some displaying a range in orientation. Part of the difficulty was caused by thermal expansion of the tantalum strip as it was held between fixed supports. However, in a different arrangement with the tantalum freely suspended in a tantalum can, high-frequency induction heating in vacuo at about l0-6 Torr produced

Jan 1, 1964

Following the suggestion of Engineering Council and at the direction of, the President, representatives from each of the Federal Government bureaus interested in map-making were called into a conference for the purpose of coordinating all of the Government's map-making activities. This conference has now reported back to the President the results of its findings, which indicate that Engineering Council's recommendation in this matter was well founded. While the conference report states that its members were of the opinion that little duplication of effort existed, it recommends the formation of a permanent Board of Surveys and Maps. An extended review of the map-making activities, which is given as an appendix to the report, indicates that this recommendation is a logical step. The conference recommendations concerning this Board of Surveys and Maps are as follows: (1) the Board is to he com-posed of representatives of mapping bureaus to be assisted by outside engineering organizations, which have been named above; (2) the estab-lishment of an information office in one of the Government bureaus, preferably the Geological Survey, which is to be under the supervision of the Board and is to be a mapping information clearing house for the Government and outside engineering organizations; (3) copyright laws are to be so changed that copies of all. maps made in the United States and with Governmental authority, will go to the central information office; (4) the Government departments are to receive orders to cooperate, with the Board; (5) future topographic maps of all kinds are to conform with specifications for the standard topographic map; (6) the U. S. Coast and Geodetic Survey to have supervision of final adjustment of all important control data under specifications approved by Board of Surveys and Maps; (7) surveys in the form of maps and publications are to be issued as soon as possible after field work has been completed; (8) program of the Interdepartmental Committee on Aerial Surveying was approved. Outside technical and scientific organizations that are called in for consultation are to operate in an advisory capacity only, responsibility for action on Governmental work is. to rest solely with the Governmental agencies.

Jan 12, 1919

By J. Parke Channing

WE are accustomed to think that we are efficient in the United States, particularly with respect to such things as mining and manufacturing. The conduct of the war has demanded in England and in France a complete readjustment of manufacturing methods and plans, and today England is probably as efficient a country as there is in the world, not even excepting Germany. This is all the more remarkable because it has been notorious for years that England has been inefficient in her manufacturing and the country has been flooded with things "Made in Germany." Today England is almost a socialistic community and the State is doing almost everything. England is now in such a position that practically everyone in the country is engaged in industry necessary for the conduct of the war, and this has been accomplished by increasing the efficiency both of her tools and of her man power. In the United States we certainly have been efficient so far as machines and perhaps so far as methods have been concerned, but we have not been efficient iii the utilization of our man power. Before the war, our labor was undoubtedly far more efficient than that of England, but it certainly was not so highly efficient as it should have been, and the problem that confronts us today, and will all the more confront us after the war, is to make our man power efficient. England has had a taste of what you may call State Socialism, and her laboring men are not going to be content to return to the old order of things. There is one feature of the labor problem in England which has permitted her to reach this condition of state socialism with comparative rapidity; this is that practically all of her laborers are English; she has little or no foreign population. While an Englishman may he a strong union man and ready to fight his employer tooth and nail, at heart he is still a British subject, and when his country was in danger he rose to the occasion.

Jan 5, 1918

By E. I. Salkovitz, F. W. von Batchelder

DURING the last few years several papers1-' have been published in which internal friction measurements have been used to determine the quantity of carbon or nitrogen dissolved in a iron. This method is based on the fact that, in pure Fe-N and Fe-C alloys, nitrogen and carbon cause peaks in the internal friction vs. temperature curve; at a frequency of 1 cycle per sec (cps) these peaks appear at $-200 and +360C, respectively, and if internal friction is expressed as Q-1, which is equal to times the logarithmic decrement, this figure will, by coincidence, give the weight percentage of nitrogen or carbon in solid solution.' In most of the studies published, very pure iron (Puron) was used. In one case the influence of manganese on the behavior of nitrogen in a iron was mentioned.4 It would be of great value, especially for the study of aging and related phenomena, if this method could be applied to commercial mild steel with norrnal percentages of manganese, phosphorus, sulphur, etc. As a rule, in such steels carbon and nitrogen are present together, and the amounts of these elements in solid solution should preferably be determined separately. The fact that their internal friction peaks appear at different temperatures (+36° and + 20°C in pure iron) seems promising for such a selective determination. It is necessary, however, that the peaks are narrow enough not to interfere with one another, and further, that there is no effect from carbon on the behavior of nitrogen in stress induced diffusion, and vice versa. According to Fast,' however, in the presence of manganese the nitrogen peak gets wider and appears at a higher temperature nearer the carbon peak, and thus the prospects for selective determination are reduced. (The carbon peak was not affected by the presence of manganese.) But even if fully quantitative de- terminations of the two elements are not attained, some relative figures on the sum of them and an indication of which one is the predominant one, would be of value. Some results from experiments along these lines will be reported here. An internal friction measuring device was assembled mainly following a description by KG." The measurements were also carried out as reported in that paper. Table I gives the chemical compositions of the four different materials used in this investigation. All materials were drawn to wires with diameter about 0.8 mm, and the analyses refer to these final shapes. Determination of Nitrogen Peak Wires from steels A, B, and C were decarburized in wet hydrogen (about 30 pct H2O) at 700°C until no carbon or nitrogen could be found by chemical analysis. No peak was then found in the internal friction. The wires were further annealed at 580°C for 16 hr in hydrogen bubbled through a solution of 6.8 pct NH3 in distilled water. Chemical analyses gave 0.04 pct N in A and C, and 0.06 pct in B. After annealing at 580°C for 15 min in a lead bath and water quenching, the internal friction was immediately measured. The resulting curves are shown in Fig. 1. At these high values of the internal friction the accuracy is comparatively poor; at Q-1 - 0.030 it is estimated to be 0.002. In order to make possible a calculation of the activation energy for diffusion of nitrogen, measurements were made at two different frequencies. Steel A shows rather broad peaks, and their temperatures can hardly be expected to be very accurate. Steels B and especially C are better in this respect. The finding of Fast' that manganese broadens the nitrogen peak is con-

Jan 1, 1953

By L. G. Huntley

A description f the geology and conditions affecting the occurrence and mining of oil; also the prospects of obtaining oil in different parts of the country. THE Colombian highlands consist of three parallel mountain ranges (Fig. 1) called respectively the eastern, central, and western cordillera of the Andes. A segment of the range that forms the backbone of the Isthmus of Panama also extends into Colombia, along the Pacific coast, as far southward as the mouth of the San Juan River. These four mountain ranges furnish the key to the varying climatic conditions and vegetation of the country. The river valleys are hot and covered with dense tropical growth. This is also generally true of the coastal plain, although in the northern portion there are some fairly open stretches where cattle are raised and even small districts where semi-arid conditions prevail. The population of this heavily wooded wet lowland depends almost entirely on river transportation for all intercourse. The elevated mountainous plateaus of the three ranges are more open and more generally cultivated; all traffic is by means of horses, mules, and the burro. The canoe and river-steamer transportation systems of the valleys are connected with the highland system of trails and roads by short cross trails and the few short railroads of the country. As these cross trails must pass through the intermediate foot-hill region, where the heavy rainfall reaches its maximum, they are exceedingly bad and the life of pack animals is short. The oil development of the Magdalena River valley is in this intermediate region, between the river and the sierras, north of Bogotá.

Jan 9, 1922

By D. D. Pollock

Many constitution diagrams do not indicate the limits oJ solid solubility of the silver-rich solid solutions below 200°C. Thermoelectric measurements were employed to determine this limit in the nieighborhood of room temperature. The appearance of a second phase causes a discontinuity to occur in the tkevtrroelectric power as a function of cornposition at constant temperature and pressure. This discontinuity was employed to determine the limits of the silver-rich terzinal solid solutions of the Ag-A l, Ag-As, Ag- Bi, Ag--Ge, Ag-In, Ag-Pb, Ag-Sb, and Ag-Sn systenls at 30°C. CONSIDERABLE work has been done on the constitution of binary alloys of silver. The available data have been compiled by Hansen1 and Elliott.2 However, many of the binary diagrams do not show the limits of solid solubility of the silver-rich solutions below about 200° C. This work was undertaken in an attempt to extend these limits to the neighborhood of room temperature . PREPARATION OF ALLOYS All of the alloys were made with silver containing less than 0.014 pct (by weight) of impurities. The materials were weighed out into 225-g heats and melted in a high-frequency induction furnace. The indium, tin, and antimony alloys were melted in A1203 crucibles, under a boric anhydride cover, and were poured into split graphite finger molds. The aluminum, germanium, arsenic, lead, and bismuth alloys were melted in machined graphite crucibles; they were also covered with boric anhydride and poured into split graphite finger molds. The $-in.-diam ingots were heated to 750°C and were forged and hot-rolled down to 0.1 by 0.1 in. The wires were pickled in a 25 pct HNO3-75 pct H2O solution to remove any oxygen-rich surfaces. The wires were then annealed at 550°C for 2 hr in a dissociated ammonia atmosphere. They were then furnace-cooled for 20 hr to room temperature in this atmosphere. The wires were cold-drawn to 0.0808 in. diam. The finished wires were again annealed at 550°C in the same manner as in the first anneal. Thermoelectric Power. The thermoelectric power of a single specimen of each alloy was determined against pure silver which contained a maximum impurity content of 0.014 pct by weight. The wire specimens were straightened and then cleaned with ethyl alcohol. They were then reannealed in the same way as the finished wires to assure that any residual stress would be at a minimum level. Previous work has shown that the presence of small amounts of stress has the effect of decreasing the thermoelectric power. The alloy specimen was soldered to the pure silver wire to form the measuring junction. A standard set of copper leads was then soldered to the reference junctions of the thermocouple. These junctions were maintained in separate dewar flasks which contained finely shaved melting ice during the test. The thermal electromotive forces of the thermocouples were measured at four temperatures between 15° and 45°C. A known source of electromotive force was balanced against the output of the thermocouple until a null balance was reached. The data were then expressed in terms of the thermoelectric power at 30°C. The results were then converted to absolute thermoelectric power, s303.3 These data have an average error of less than ±0.2 pct. RESULTS AND DISCUSSION All of the experimental data are given in Table 11. Since the electromotive forces of the binary alloys of silver were determined against the pure silver from which they were made, the resultant thermoelectric powers are only a function of the intentionally added binary elements at the constant test temperatures. This provides a direct measure of the effects of the alloying elements. The absolute thermoelectric power of an alloy of silver is given4 by:

Jan 1, 1968

By M. L. Hammond, G. M. Bowers

Silicon dioxide films have been prepared on silicon wafers by the oxidation of SiH, near 400°C. Results previously reported by Goldsmith and Kern7 have been qualitatively corrobovated using a system of different geometry, and significantly greater deposition rates have been achieved. The deposition rate is independent of thickness and nearly independent of the O2/SiH, ratio over a wide range; however, the rate is strongly temperature-dependent. The structure of the deposit depends upon the cleanliness of the substrate, and the electrical field strength of the deposited oxide depends upon the nature of the electrodes. MULTILEVEL interconnects in integrated circuits using aluminum metallization require an insulator that can be deposited at low temperature. Because the A1-Si eutectic is only 577°C, the maximum deposition temperature must be below about 500°C to prevent reaction of the aluminum with the silicon and with other materials in the integrated circuit. Many methods of depositing insulating films of SiO, and other dielectrics have been reported'-6 but the technique described by Goldsmith and Kern7 offers the simplest method of preparing SiO, films. The technique involves the reaction of SiH, and 0, to form SiO, films in the 300" to 500°C temperature range. Previous work using this gas system has been reported8 and the initial development work at Philco Microelectronics was done at the East Coast R&D Laboratories. 9 This paper corroborates some of the results of Goldsmith and Kern,7 shows that much higher deposition rates can be obtained than previously reported, and presents some observations on the structure of deposited SiO, films. EXPERIMENTAL CONDITIONS Fig. 1 is a schematic drawing of the apparatus used in this study. It differs from that of Goldsmith and Kern in that 1) the gases are mixed before they enter the reaction chamber, 2) there is no fritted glass diffuser, and 3) the wafers are stationary during deposition. The control thermocouple was in a well located 0.06-in. from the substrate, and three gas supplies were used: 1 pct SiH4 in N 2, O 2, and N 2. Water vapor must be excluded from the plumbing to prevent the formation of colloidal SiO, and the SiH4 must be diluted with an inert gas because SiH4-0, mixtures are extremely flammable above about 4 pct SiH The wafer temperature was determined by attaching a thermocouple to a test wafer and the temperature was maintained to +5 C. The conditions used in this investigation are listed in Table I. The temperature range was chosen for compatibility with the A1-Si system. The volume ratio of 0, to SiH4 is the actual volume of 0, delivered to that of SiH4, taking into account the initial dilution of the SiH4. This ratio, which was used by Goldsmith and Kern,7 is a useful indicator of the experimental conditions. The active/inactive ratio is the ratio of the volume of active gases, SiH4 and O2, delivered to the volume of dilution gas. The active/inactive ratio is an important parameter to specify for deposition rate determinations since it determines the amounts of reactants that arrive at the sample per unit time. Fairly high dilution ratios were necessary to achieve uniform deposits of SiO,. Most of the process characterizations were performed on the polished (111) face of 3 to 5 ohm-cm, n-type silicon wafers which were 0.009 in. thick; but the data approximately apply to deposition of SiO, on thin films of aluminum. It is difficult to obtain accurate deposition rate data over aluminum films because of coarsening the aluminum surface during exposure to 300" to 400°C. The deposited SiO, film fol-

Jan 1, 1969

By B. F. Decker, J. H. Keeler, W. R. Hibbard

Textures of hot-rolled, of cold-rolled, and of cold-rolled and annealed zirconium sheets were determined by use of an X-ray spectrogoniometer. All textures showed a tilt of the basal planes 240" from the rolling plane about the rolling direction. Deformation textures showed the [1010] direction to be approximately in the rolling direction. After recrystalliza-tion, the 111201 direction was approximately in the rolling direction. This texture was sharpened by annealing above the allotropic transformation. Textures of sheet produced by alternately cold rolling and then annealing were less strongly oriented than sheets that underwent severe deformation without intermediate anneals. THIS study of the deformation and annealing textures of high purity zirconium was carried out to supplement an investigation of zirconium and zirconium-base alloys. The spectrogoniometer method of pole figure determination was used and yielded more detailed and precise information than the photographic techniques used by previous investigators. Earlier investigations of the rolling textures of hexagonal metals titanium,1,2 beryllium," and zirconiumL having a c/a ratio slightly less than 1.6 disclosed a rotation of the basal planes from the rolling plane about the rolling direction so that the basal poles were inclined toward the transverse direction, and with one exception,& the [1010] direction was found parallel to the rolling direction. Similarly, hot rolling produced a spread of the basal poles in the transverse direction,2,3,5 With the [1010] direction parallel to the rolling direction. The textures of these metals after recrystallization differ somewhat from each other although still exhibiting the transverse rotation of the basal poles about the rolling direction. Zirconium" was found to have the [1120] direction in the rolling direction, beryllium" continued to have the [1010] direction in the rolling direction, and titanium' was shown to have the [1010] direction in the rolling direction (the cold-rolling texture) when annealed at 1000°F, changing to the [1120] direction in the rolling direction when annealed at 1500°F. It was suggested2 that the titanium retains the deformation texture after re-crystallization, and preferred grain growth at higher temperatures produces the second texture. Annealing above the allotropic transformation temperature did not appreciably change the high temperature recrystallization texture for titanium.' Coarsegrained zirconium showed more spread" in the transformation texture than in the recrystallization texture. The material used in this investigation was crystal-bar zirconium prepared by the iodide process. The major impurity was hafnium which was less than 0.3 pct. The composition obtained by spectro-graphic analysis is given in Table I. The hot-rolled specimen was prepared from a 50-g button of zirconium arc-melted in a water-cooled crucible under an argon atmosphere. This button was enclosed in a welded sheath of soft iron and the ensemble was rolled at 825°C. After each pass the sheath was put back into the furnace to allow it to return to the desired temperature. The zirconium ingot was reduced in this manner to a thickness of about 0.035 in., a reduction of approximately 90 pct. The sheet after removal from the sheath was alternately polished and etched to a thickness of 0.001 in. Cold-rolled specimens were prepared from crystal bar by a series of reductions of approximately 0.010 in. until the sheet reached a thickness of 0.010 in. after which it was cold-rolled to 0.001 in. thickness between sheets of alloy steel. The total cold reduction amounted to about 99.8 pct. Specimens were annealed in an evacuated Vycor or quartz tube. The transmission pole figures were obtained by the quantitative method of Decker, Asp, and Harker6 modified by Geisler7 using an X-ray spectrogoniometer with Cu Ka radiation. Unless otherwise specified all four quadrants were examined with 5" increments along the radius of the pole figure. Absorption corrections were made for changes in length of the X-ray path through the sample as inclination of the

Jan 1, 1954

By Byron W. Cheever

In working up the process which I described at the Chicago Meeting, May, 1884 (p. 163 of the present volume), for the estimation of phosphorus in iron and steel, I employed samples of steel obtained from one works only, and of a given brand. Since then I have had frequent occasion to test the process on other steels, and find that it works equally well. But some steels present certain colors which may mislead the operator; and I therefore propose a slight change in the directions formerly given. On the second page of my paper, in the second paragraph, I would substitute the following modified directions: Place the flask under the hydrant, till the solution is perfectly cold ; then add, gradually, strong ammonia, with constant stirring, till the solution is changed into a pasty mass and the ammonia is in slight excess; then add cautiously HNO3 (1.40 specific gravity)

Jan 1, 1885

By Arthur F. Taggart

In 1900, Elmore found that if an acidulated pulp was stirred up with an oil which was relatively insoluble in and lighter than water, and the mixture was allowed to stratify, much of the sulfide would be found hanging to the lower surface of the floating body of oil and could be skimmed off or overflowed with it. The action of the flotation agent here is twofold, first to select the sulfide from the gangue—what today is called collection—and second, to buoy the collected sulfide away from the gangue. The action in collecting is illustrated by Fig. 1: which contrasts the behavior of drops of oil brought, under water, to the surfaces of gangue and sulfide particles, respectively. The oil displaces water from the surface of the sulfide; the water displaces oil from the gangue surface. If, instead of considering the solid particles the fixed parts of the system of oil, water and solids. we consider the oil and water fixed and the solids presented to the surface of contact, the condition will be as shown in Fig. 2; the sulfide tends to be drawn into the interface and the gangue to be excluded. The sulfide particles are held in the oil-water surface by the tension of this surface. The buoyant effect is supplied by the oil droplets in bringing the sulfides to the water surface, but not in holding them there. Gas as Buoyant Medium of Flotation In 1906 Sulman. Picard and Ballot discovered a practical and substantially fool-proof method of doing what Everson, in 1886, and Fro-nlcnt. DeBavay Bessel and Elmore had been doing in the intervening years, viz.: using gas in place of oil as the buoyant medium for flotation, but retaining oil as the agent. To all of these inventors "oil," with no qualification as to its kind and no true understanding of its function, was the important thing. Hut they placed on the oil an additional burden viz.: froth-making, and it soon became apparent that not all oils were suitable for the dual purpose. As a matter of fact, it is probable that each of these inventors knew only one suitable oil at the time he wrote his patent, but used the generic term in the patent with the usual idea

Jan 1, 1928

By N. S. Stoloff, R. C. Ku, R. G. Davies

The stress-strain behavior of Fe-Co and Fe- V alloys containing up to 25 pct solute have been studied in the temperature range 25° to - 196°C. The microyield stress is independent of temperature for all alloys studied, while the temperature dependence of the ordinary yield stress is large and comparable to that for unalloyed iron. An alloy-softening phenomenon is observed for many alloys relative to unalloyed iron, and appears to be a consequence of removal of inter-stitials from solution and their subsequent agglomeration. The ductile to brittle transition temperature is increased markedly by both cobalt and vanadium. Transmission electron microscopy observations reveal that cross slip and cell formation are restricted with increasing solute, which can account for many aspects of yielding and fracture behavior. IRON and other metals of bcc structure slip on many planes of the (111) zone at moderate and elevated temperatures, giving rise to wavy glide. At low temperatures, however, there is a tendency for slip to be restricted to planes of only one or two crystallographic types; in the case of Fe-Si alloys for example, (110) glide predominates, giving rise to planar slip bands."' Restriction of cross slip at low temperatures in iron has been linked by Brown and Ekvall3 to increased strain hardening in the preyield microstrain region, leading to an apparently large temperature dependence of the yield stress. Support for this view has been provided by Lawley and Gaigher4 from a transmission electron microscope study of molybdenum. They concluded that dislocations at lower temperatures, by virtue of their inability to change planes readily, are unable to interact and annihilate, leading to an increase in internal stress and work-hardening capacity. Restriction of cross slip at low temperatures has also been suggested to be an important factor in determining the ductile to brittle transition of single-phase solids, including metals of bcc structure.5 It is pertinent to note that most solute elements tend to raise the ductile to brittle transition temperature of poly crystalline ferrite,6,7 although in some cases, e.g., Fe-Cr7 and Fe-Al,8 the dilute alloys may actually yield at lower stresses than unalloyed iron. It appears, therefore, that solute elements may have an effect analogous to lowering the test temperature with regard to restricting cross glide. Such an effect has indeed been observed in the ionic alloy system KCl-KBr,9 in which bromine atoms, although causing little misfit and consequently little effect on the yield stress of KC1, have a pronounced effect in restricting wavy glide and inducing brittleness. The purpose of the present investigation was to determine the effects of selected solute atoms on the yield stress and fracture behavior of iron, and to elucidate in turn how the slip character was related to these properties. Since it is known that interstitial atoms exert a strong influence on the mechanical behavior of iron, the solute elements chosen for study were vanadium, which reacts strong with interstitials,10 and cobalt, which does not form highly stable interstitial compounds." EXPERIMENTAL PROCEDURE Four-pound ingots of each of the following alloys were vacuum-melted in zirconia crucibles: Fe-1, 5, 10, 25 at. pct Co, and Fe-1, 4, 10, 20 at. pct V. An ingot of unalloyed iron from the same original stock as that used for the alloy was remelted under similar conditions to eliminate variations in interstitial content arising from differing thermal histories. Chemical analyses of the iron, cobalt, and vanadium melt stock are listed in Table I. All ingots were rolled and swaged, commencing at 850°C, to 1/4-in.-diameter bar. The bars were then annealed at 850°C for 1 hr (except that the 10 and 20 pct V alloys were heated for 2 hr) to give a uniform equiaxed grain size of about 0.05 mm. Tensile samples of 0.125 in. diameter by 0.8 in. gage length were utilized for studies of the ductile to brittle transition. A second set of tensile samples were utilized for microstrain experiments in which strain sensitivity of 1 x 10"6 was achieved by a capacitance method.3 Cylindrical compression samples 0.250 in. diameter by 0.4 in. long also were prepared to study the influence of composition on the macroscopic yield stress, and for metallographic analyses of defor-

Jan 1, 1965

Jan 1, 1958

Not many accounts of mining methods or labor conditions in the mines in early days can be found; all that have seemed to be authentic have been included in the preceding chapters. In practically every field opened before 18.10 the first coal was recovered by quarrying, or strip mining, the operations, of course, being by hand and on a very small scale; new places were opened as soon as mining became difficult or expensive. Where it became necessary to drift into the hillsides, the first coal was taken out by sleds, and later by small wagons, the power being supplied by the miner, often assisted by dogs. Wooden rails then came into use with small cars running on them. These cars were very small, usually holding only a few bushels; in the Belleville, Illinois field as late as 1863 cars having capacities of 10, 12, 14 and some as large as 30 bushels were in use. It was not until late in the 1830's that horses or mules came into use for haulage purposes in the Pittsburgh region, although some had been used in the Richmond, Virginia field at an earlier date. Coal was usually undercut by hand and wedged down, until explosives came into general use, and in nearly every field the coal was forked into the cars, the fine coal, or slack, being left in the mine. Hours worked were very long, but few records remain to show what they were at different places and times; there was undoubtedly a great variation between districts and mines. Roy stated a miner could often produce 5 or 6 tons in a day of 8 or 9 hours in a 5 or 6 foot seam, but in another seam possibly could mine only 3 1/2 to 4 tons. He estimated an average day's work in a four foot seam at about 3 1/2 tons.1 In a strike in the Belleville field in 1863 it was found that an average skilled miner in the field could probably produce 4 to 5 tons a day.2 This was only the coarse coal loaded and did not include slack. In 1873, a coal undercutting machine was tried at a mine about two miles from Brazil, Indiana, said to be the first coal machine ever invented in the United States. It was run by a 5 H.P. steam engine (later to be changed to compressed air), and consisted of an iron rim, four feet in diameter with movable steel teeth placed about one foot apart. The rim

Jan 1, 1942