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By Robert E. Barieau

A list of 163 references to original experimental PVT data on helium is presented for the period 1895 to 1968. The list is complete as of the start of the Helium Centennial Year, 1968, to the best of the author's knowledge. Citations were keypunched for easy updating and are listed alphabetically by author.

Jan 1, 1968

By Sabri Ergun

This report gives the result of investigations of coals of different rank, coal com¬ponents, chemically and thermally treated and irradiated coals, and sedimented organic matter. In most studies the arbitrary parameters obtained from the usual quantitative profile analyses are not given largely because they lack physical meaning. Instead comp interpretations are offered. X-ray patterns of high-volatile bituminous and lower rank coals are not self¬-sufficient for structural interpretation by the methods of analysis developed to date. The patterns of hydrogenated and dehydrogenated coals indicate that the basic change in the structure of bituminous coals with increase in rank is the conversion of alicyclic structures into aromatic layers. In low-rank anthracites the aromatic layers are about 10 A in size. The increase in rank is the result of coalescence of layers. High-rank anthracites have layer sizes of 25 to 40 A and exhibit the development of three-dimensional (hkl) reflections of graphite, indicating ordering of adjacent layers. In meta-anthracites the layers are > 1000 A and the basic structure is that of defective crystalline graphite. The well-known petrographic components in low-rank coals have different structures; the differences dissappear in low-volatile bituminous and higher rank coals. The patterns of sedimented organic matter, except impsonites, differ from those of coal hydrogen contents are high, and their X-ray patterns are consistent with those of structures. In contrast to normal coals, the patterns of uranium-bearing coals show increased diffuseness with decrease in hydrogen content. The diffuseness is accompanied by increase in the uranium content of the coal. It is very likely that high uranium-bearing coals have predominantly tetrahedral structures.

Jan 1, 1968

By Ralph W. Marsden

The natural iron ores of the Lake Superior Region in the United States are being replaced by iron-ore concentrates produced from magnetite- or hematite-rich horizons in the Precambrian cherty iron formations. The production of natural ores will soon be less than one-half of the total ore shipped annually. The tonnage of natural ore produced will continue to decline until it is a minor percentage of the ore shipped. The natural ores include (1) soft ore, (2) hard ore, ( 3) conglomerate ore and ( 4) siliceous ore. The soft ores are the important ore type and are sometimes termed "Lake Superior type ore". These ores are in situ deposits of hematite and limonite formed by the leaching of silica and other gangue materials in the iron formations. The leaching is believed to have been done by downward moving surface waters. In deep ore deposits, generally over 1000 feet below the present surface, circulation and leaching action may have been assisted by hydrothermal activity. Hard ore deposits occur on the Vermilion and Marquette ranges where hematite or magnetite has replaced the silica (and possibly some silicates) in cherty iron formation. These ores commonly occur in structural situations favorable for the movement of hydrothermal waters. The ores are believed to be the result of hydrothermal action with iron, possibly from the iron formation, transported by hydrothermal waters to areas favorable for the replacement of silica by iron oxides. Certain stratigraphic horizons of the Lake Superior Precambrian cherty iron formations contain sufficient iron as magnetite or hematite, with a grain size and texture that will give adequate mineral liberation, to yield an ore-quality product after grinding and concentration. The magnetite-rich deposits are termed magnetite taconites. These ores occur on the Mesabi, Gogebic, and Marquette ranges. Magnetite taconite ores are unenriched cherty iron formation and are the result of the sedimentary deposition of the iron formation and the metamorphic history of the rock. The commercial quality hematite-rich iron formations in Michigan are termed jasper ores. The jasper ores are being mined on the Marquette and Menominee ranges. These ores are composed of specular or granular hematite associated with quartz and iron silicates. The jasper ores appear to be recrystallized iron formations in which iron, prior to recrystallization, occurred as hematite.

Jan 1, 1968

By Frank G. Snyder, Paul E. Gerdemann

The Southeast Missouri lead district, located about 70 miles south of St. Louis, embraces four important sub-districts and several minor ones. The important sub-districts, in order of discovery, are Mine La Motte, the Old Lead Belt, Indian Creek, and the Viburnum Lead Belt. Descriptions that follow are of geology and ore deposits of the Old Lead Belt. The ore deposits are stratiform in character and are localized in a narrow carbonate bar and algal reef environment on the flanks of exposed Precambrian of the St. Francois Mountains. Ore structures include a variety of primary depositional features such as pinchout zones, disconformities, ridge structures, reefs, and submarine gravity slides. Faulting, prior to and during ore deposition, "prepared" the host rock and strongly fractured areas are mineralized much more intensively and extensively than unfractured parts of the same sedimentary structures. The deposits are epigenetic in character. Mineralization is believed to have occurred at the time that post-lower Ordovician faulting took place. The mineralizing solutions are believed to be concentrated brines from adjacent basins that moved out of the basins during faulting, uplift, and erosion of the St. Francois positive area.

Jan 1, 1968

By Samuel M. Brock

Problems related to strip and auger coal mining have grown with the development of the industry and the economy. New technology has produced equipment that has made mining by surface methods not only highly productive, but potentially highly destructive of water resources and natural environments. On the other hand, growth of the economy has produced an increased demand for clean water, and created new demands for amenity values that natural environments provide. Thus, opposing forces have created conflicts in resource use. And these conflicts have made surface mining highly controversial. Resolving the controversy will require the solving of complex economic and social problems. The essence of the economic problem created by surface mining is that, in the absence of proper regulation, substantial costs resulting from the process are borne by the public rather than the mine operator.

Jan 1, 1968

By I. J. Hegyi, J. J. Tietjen, H. Nelson, J. I. Pankove

The fabrication of p-n junctions in GaAsl-,P, alloys by a vapor-phase gowth technique has for the first tirne resulted in room-temperature injection lasers capable of operating over a broad range of wavelengths extending into the visible region of the spectrum. The shortest wavelength achieved to date is 6750A at room tetnperature. In addition, at 78°K the threshold current density values for these lasers are generally the lo~vest reported, and the emitted radiation extends to the lozc,est wavelength ever attained (6350A). With lasers fabricated from material containing 14 pct Gap, quanticm efficiencies of 26 pct and peak power outputs of 25 zu were obtained at room temperature. ALTHOUGH room-temperature operation of GaAs injection lasers has been well-documented,&apos;-5 the operation of GaAsl-,P, (x > 0) laser diodes has been restricted to relatively low temperatures.8-&apos;0 This has been previously attributed5, 7, 10-12 partially to the difficulty of preparing single-crystalline GaAsl-& alloys having a high degree of chemical homogeneity and purity. Also, with these materials it has been difficult to prepare high-quality, abrupt p-12 junctions by diffusion techniques; and, in turn, this has made it difficult to obtain optimum electrical properties for room-temperature operationL3 in the resulting laser diodes. As a result, GaAsl-,P, laser diodes have not been efficient enough to permit operation at room temperature. For example, using diffused structures, only a few diodes were obtained which could be operated even close to room temperature (255K)." Recently, a vapor-phase growth method of preparing epitaxial deposits of GaAsl - .P, alloys has been described,14 and the high-purity and homogeneity of these materials has been previously demonstrated. Of special significance, with this technique, n- or p -type doping can be initiated or discontinued at any time and at almost any rate during the crystal growth so that the donor and the acceptor concentrations can be easily controlled to obtain desired impurity profiles. This permits high-quality, abrupt p-TZ junctions to be vapor-phase grown entirely during the crystal growth process, so that diffusion or other p-n junction fabrication processes are unnecessary. After growth, the device does not have to be heated to elevated temperatures, which avoids the possible unwanted introduction and motion of both impurities and lattice defects. Using the vapor-phase growth method cited above, over 300 room-temperature injection lasers have been prepared from GaAsl-,P, alloys having compositions in the range of 0 5 x 5 0.41. These lasers have emitted cohe~ent radiation in the spectral range of 8350 to 6350A at 78°K or from 9000 to 6750A at room temperature. The threshold current densities of the best lasers are independent of the alloy composition over the range 0 < x < 0.2 and compare favorably with values for good GaAs lasers.&apos; MATERIAL PREPARATION Multilayer, epitaxial deposits of GaAsl-,P, alloys are prepared by a vapor-growth technique described elsewhere.14 With this technique, the individual layers which comprise the multilayer structure are prepared sequentially in the deposition apparatus without interrupting the crystal growth. The epitaxial layers are deposited on GaAs substrate surfaces oriented normal to the ( 100) direction. The substrate wafers employed in this study were usually doped with tellurium to an electron concentration of approximately 2 x 10" per cu cm. To avoid strains, the first 10 to 15 p of the deposited material is uniformly graded from pure GaAs to the specific GaAsl- ,P, alloy composition of interest. The GaAsl - ,P, alloy growth is then continued to form a layer of constant composition having a thickness in the range of 25 to 75 p. Both the graded region and the layer of constant composition are doped with selenium to an electron concentration of about 2 x 10" per cu cm. The p region of the diode is then incorporated in the crystal by abruptly changing the dopant concentrations in the vapor phase to facilitate doping with zinc. This layer has a hole concentration of approximately 3 X 1019 per cu cm and typically is 50 p thick. DEVICE FABRICATION In general, the GaAs substrate and the region of graded composition are removed. Ohmic contacts are made to the n-type side by tin evaporation and to the p-type side by an electrodeless nickel deposition. This is followed by an electrodeless deposition of gold on both sides. The crystal wafer is then cleaved along (110) planes and sawed into rectangular parallelepipeds. Typical dimensions are 100 by 300 for the junction area and 100 µ for the diode height. The diodes are either soldered to a copper stud or pressure-mounted in a copper clip. RESULTS AND DISCUSSION Approximately 400 laser diodes having compositions in the range of 0.41 have been prepared by the method described above. Each laser was routinely tested at liquid-nitrogen temperature. The lasers were operated with l-psec current pulses at a repetition rate of 60 pulses per sec. The parameters of greatest practical interest are the photon energy or wavelength of the laser output and the threshold current density. Fig. 1 shows the variation of photon energy with alloy composition at 78°K. The composition was determined from the lattice constant of the material obtained by X-ray back-reflection measurements. Although there

Jan 1, 1968

By Thomas M. Nasiatka

This report briefly describes the present state of the art and the technological highlights of tunneling from its inception to the present. The discussion is concerned primarily with tunnels driven through relatively competent rock for mine development and various civil purposes. In addition to pinpointing the major technological breakthroughs in tunneling, this report indicates their general effect on the speed of tunneling. The tunneling speeds are based upon data from approximately 80 tunnels listed in the appendix. These data include length; cross section shape and dimension; type of rock; tunneling method; method of breaking, loading, and transporting the rock; average linear progress rate; and cost in values during the period of construction. Most of the tunnels described have diameters of 15 to 30 feet.

Jan 1, 1968

By Theodore J. Williams

Computer control has been one of the fastest moving and most glamorous fields of industrial development in the past decade. A review of this period shows some truly remarkable accomplishments in both system development and applications. In addition, work now under way promises results which will continue the rate of progress of the past. This paper will review the history and status of the field of computer control and point out the major breakthroughs which have occurred. It will analyze the present trends and extrapolate them to predict the early future developments in the field.

Jan 1, 1968

By Paul Wellman

A computer program is presented that may be used to calculate the bare equipment cost of the major processing units for any hot potassium carbonate gas purification system. The program is designed such that, with only minor modifications, it could be used with a variety of computer systems.

Jan 1, 1968

By J. F. Held

In a study of the influence of cold rolling on mechani cal properties of steel, it was found that the specific rolling procedure influenced crystallographic orientation. Properties developed by several rolling modes were determined and related to crystallographic orientation. Sanzples were cold-rolled various amounts on a laboratory mill. When palm oil was used as a lubricant, the crystallographic orientation was homogeneous throughout the thickness of the samples. Other samples were rolled without lubrication. Variations in intensity of the recrystallization texture components persisted throughout more than 50 pct of the volume of these samples. When the average plastic strain ratio, which is dependent upon crystallogvaphic orientation, was plotted as a function of percent reduction, a maximum was found at 40 pct in the samples which contained the observed texture variation. No maximum was found for the samples with the homogeneous texture distribution. Other mechanical properties, such as tensile strength and yield strength, were not influenced by the variation in crystallopaphic orientation. MECHANICAL properties of steel sheets depend, in general, upon the structural properties of the steel. For example, the Petch equation describes the relationship between yield strength and grain size. Other properties, such as hardness, vary with chemical composition. The plastic strain ratio, or R value, has been found to be dependent upon crystallographic orientation . In the course of investigating the effect of cold rolling on mechanical properties, it was found that a previously reported relationship between percent cold reduction and R value was not always observed. Published data had shown that the optimum cold reduction for best R values is 70 pct for aluminum killed steel.&apos; However, by altering the rolling conditions, the optimum reduction can be shifted to much lower values, or it can be moved to very high values. This paper describes the rolling conditions that lead to shifting of the optimum cold reduction. The effect of rolling conditions on the various structure parameters and the resulting mechanical properties are evaluated. EXPERIMENTAL PROCEDURE Samples of three low-carbon aluminum killed steels were cold-rolled various amounts on a 9-in.-diam 2-high laboratory mill. Hot-mill thermal practice and steel chemistries are listed in Table I. Steel A was rolled with palm oil lubrication and heavy reductions on each pass; i.e., a total reduction of 75 pct was ac- complished with a maximum of five passes. Steel B was rolled without lubrication, and light reductions were given on each pass. After approximately 75 pct reduction, it was necessary to use a small amount of light oil to achieve any additional reduction in thickness. Following cold reduction, the samples were box-annealed at 1300°F for 10 hr. The heating rate between 800" and 1300°F was 50°F per hr, and the cooling rate following the soak period was 50°F per hr. Tensile specimens were machined from the annealed material and these were used to measure yield strength, tensile strength, and the plastic strain ratio (R value). Recrystallization textures were determined by an inverse pole figure technique.*&apos;3 Integrated intensities of the (110), (002), (112), and (222) reflections were recorded for those planes lying parallel to the sheet surface. Examinations were made on both surfaces of each sample, and also at various levels beneath each surface to approximately 0.010 in. depth by etching techniques. RESULTS R Values. The R values obtained in steels A and B are shown as a function of percent cold reduction in Fig. 1. No optimum cold reduction was observed in steel A, rolled with palm oil lubrication. It is likely, however, that an optimum reduction would have occurred had higher reductions than 88 pct been employed. The optimum reduction in steel B occurred at 40 pct. The behavior in both of these steels is quite

Jan 1, 1968

By W. Henry Weimer

A successful surface coal operation requires the combined efforts of engineering and operating personnel. In the planning for a mine, machines should be selected to do the best work in getting the coal uncovered, loaded, and transported to the preparation plant. The best system and extent of cleaning will be determined by the market. After the fundamentals of operation have been established, the operating personnel should see they are carried out. There is no simple solution to some of the every day problems facing the operating officials. Here the production engineer with the technical approach, time studies, control methods, past experience, and available records can help in detecting causes of inefficient phases of the operations. With these studies, a careful analysis can be made in setting up the expected standards to be followed. Management can then compare the job under study with the standards and make corrections to solve the problems. 5.2-1. Annual or Daily Coal Production. Once the production cycle has been established, it is paramount that coal sales keep the productivity of the mine as high as possible. A successful company does this by what they call "the control approach." The daily tonnage report is one of the things that is a potent control tool in attaining the goals to be achieved. If production is falling short of the goal, the daily tonnage report will reveal what has to be done in the remaining days of the month or year to achieve the expected schedule. When goals are reached or exceeded, then budgeted tonnages and costs will be reached or exceeded and thus assure attainment of a profit. Failing to keep to the scheduled pace shows up quickly and prominently, facilitating any necessary action to get things back to the projected plans. The sales target is usually set a little higher than the operating production. The sales tonnage is scheduled and sales are made accordingly, slightly

Jan 1, 1968

By T. A. Lloyd

"This paper indicates the extent to which Canadian coal mine operators have taken advantage of developments in the science and technology of coal that would allow them to better satisfy changing market demands through improving the properties of their products. At some mines, no attempt is made to alter the coal from its as-mined condition, but at most mines grading into various size ranges and hand-cleaning of lump sizes is undertaken.Over-all, Canada Jags behind most of the other major world coal producers in the proportion of its coals being processed in wash plants. To some extent, this is due to the fact that a high proportion of the coal production satisfies market demands without such treatment. On the other hand, a few of the coal mines in Canada, which produce about 25 per cent of the nation's total coal output, have in operation some of the most modern coal beneficiating equipment available, including jigs, flotation cells, water cyclones, centrifuges, disc filters and thermal dryers."

Jan 1, 1968

By R. J. Lutton

The U. S. Army Corps of Engineers is seeking empirical slope data from mining companies and other organizations to help establish guides for engineering Judgment in crater excavation for canals and other civil works. Slopes from about 100 open pits and other excavations range in heights to greater than 1000 ft. Factors known or expected to affect stability (and optimum slope inclination) are: geological structural orientation, geological structural ordering, method and technique of blasting, design life of slope, groundwater conditions, depth of excavation, climate, and height. These and other more subtle factors appear to combine and produce an overall effect brought out best on a family of empirical curves relating slope height and inclination.

Jan 1, 1968

By R. J. Leary

This investigation was conducted to determine the effects of various rare-earth metal addition practices upon the macrostructure and the pattern of sulfur distribution in steel ingots. Heats of plain carbon steel were melted in a 1-ton, basic electric-arc furnace. Melts were treated with mixtures of rare-earth silicides, aluminum, and cryolite either in the furnace before tap or in the ladle after tap to determine the effects of this form of rare-earth treatment upon ingot macrostructure. Steels thus treated with rare earths in the furnace were characteristically free of the gross subsurface nonmetallics which typically result from conventional rare-earth treatments. Steel treated in the ladle showed only a few such nonmetallics, and practical techniques were developed for eliminating most of these. Results showed that furnace deoxidation was controlled by the concentration ratio of rare earths: aluminum. During casting, deoxidation was controlled by the concentration of rare earths. Oxygen contents equivalent to vacuum ladle degassing resulted from air-melt furnace treatments with the rare-earth mixtures described. Rare earths in steel inhibited the onset of equiaxed grain formation during ingot freezing, and also virtually prevented interdendritic segregation of sulfides.

Jan 1, 1968

By William H. Hallahan

The Friedensville zinc mine of The New Jersey Zinc Company is located about four miles south of Bethlehem, Pennsylvania in the Saucon Valley, an infolded and down faulted block of Cambro-Ordovician carbonate sediments surrounded by hills of pre-Cambrian gneiss and Cambrian quartzite except where breached by Saucon Creek at its entrance into the Lehigh River. The Beekmantown formation of lower Ordovician age is the host for zinc and limonite ores, the former occurring in the lower dolomitic portion thereof and the latter in the upper interbedded dolomite and limestone portion of the section. The Beekmantown is overlain unconformably by the Jacksonburg of middle Ordovician age and according to Miller (2) underlain conformably by about 2500 feet of Cambrian dolomites and 200 feet of the basal Cambrian Hardyston quartzite. Igneous rocks, younger than the Cambro-Ordovician carbonate rocks, are absent in the vicinity of the ore deposits. The major structure is a N60°E-trending saddle-shaped doubly plunging anticline overturned to the north. A syncline lies to the north of the anticline. A thrust fault of substantial displacement repeats the south limb of the anticline. The ore consists of sphalerite and pyrite, along with gangue dolomite and quartz, filling and replacing the sedimentary type matrix of a strata-bound solution collapse breccia in the dolomitic portion of the lower Beekmantown. This breccia was produced in pre-Jacksonburg time as a consequence of uplift, erosion, and development of a karst topography and subsurface drainage system in the Beekmantown. Deposits of both zinc and limonite are present on the vertical north limb, on the crest and on the gently dipping (25°) south limb of the Friedensville anticline; consequently, there is no preferred structural setting for mineralization. Rather this distribution supports the view that the folding is post-ore. Features confirming this view are the development of flow cleavage in the breccia matrix, the deformation of some of the sphalerite, and the fracturing of the pyrite mineralization therein. There is nothing to indicate that the age of mineralization is other than Ordovician and older than Taconic deformation. In the absence of intrusive igneous activity younger than the ore host, the writer suggests that submarine volcanic exhalations associated with the volcanic activity recorded in the eastern eugeosynclinal facies of the Ordovician may be the source of the metal ions.

Jan 1, 1968

By William S. Miska

The study is an economic evaluation of historical, current, and projected refractory uses in the iron and steel industry of the United States. The first part of the report presents a refractories classification and identifies principal trends in the refractories industry; such as, value and volume of shipments, prices of finished refractory products, the number of manufacturers and plants for refractories production and marketing. The main part of the report treats refractory use patterns and technologic developments affecting refractories usage in the iron and steel industry. Changes in use patterns in each furnace type, refractory, and installation costs and the future outlook for refractories in ironrnaking and steelmaking are covered. The last part of the report identifies the principal raw materials used in refractories production and treats trends in refractory raw material consumption. An appendix to the report contains historical time series graphs of shipments of refractory types used primarily by the iron and steel industry and principal refractory raw materials sold or used by producers. An equation of the line of best fit was calculated from the earliest to the latest year in each time series, usually 1950 to 1965; these were extrapolated in order to derive volume estimates for the year 1975.

Jan 1, 1968

By Hillary W. St. Clair

Reaction rate coefficients were determined from analyses of the effluent gas for the reduction of granular ferrous oxide to metallic iron by passing carbon monoxide through a packed bed of oxide at a controlled rate in the temperature range 1,000° to 1,300° C. Coefficients were determined by the comparison of observed analyses and calculated analyses using a mathematical model that takes into account the nonuniform composition of both the solid oxide and the gas. A method is also given for finding the value of the rate coefficient that best fits the observed data.

Jan 1, 1968

By N. A. Gjostein

The real and apparent dependence of the surface self-diffusion coefficient, Ds, of gold on crystallo-graphic orientation has been investigated by isolated scratch smoothing and grain boundary grooving experiments. No systematic variation of Ds with orientation was found along the [100] zone. In view of the experimental scatter in these results, however, only aniso-tropy ratios, p, greater than -1.3 would be detectable. Anomalously low values of Ds were found on the [0ll] and [110] zones when the diffusion direction lies along (the scratch or grain boundary groove is perpendicular to) these zones. By comparing these results with a previous y plot study of gold, it is hypothesized that this is not an intrinsic diffusivity effect, but rather it results from a decreased driving force for mass transfer at orientations where the y-plot curvature is negative and appreciable in magnitude relative to y. The characteristics of this type of anisotropy do not appear sEVERAL investigations1-7 have dealt with the anisotropy of the surface self-diffusion coefficient, Ds, of metals as measured by the decay of single or multiple to be in agreement with the hypothesis of fast diffusion along ledges in the surface structure. In certain cases the Fourier method of determining Ds, described in Paper I of this series9 was compared with the second moment analysis in order to determine whether or not the method of analysis affects the anisotropy ratio. While the type of analysis does influence the magnitude of the anisotropy ratio, this effect is not associated with the shape of the profile, but rather is connected with the iterative volume diffusion correction used in conjunction with the second moment analysis. It is further demonstrated that the volume diffusion correction can be too large by either method when the y-plot curvature effect is large. Certain orientations exhibit an unusual temperature dependence of Ds ; this is discussed in terms of the y-plot curvature effect and/or the influence of impurities on Ds . scratches in the surface. Depending on the system investigated, both large1"3&apos;6&apos;7 and small4&apos;5 anisotropies in Ds have been found. Although adsorbed impurities undoubtedly play an important role in determining the magnitude of the anisotropy,8 there are other factors that can give rise to an apparent anisotropy in Ds, thus obscuring the true nature of an intrinsic anisotropy in

Jan 1, 1968

By F. W. Wood

The use of consumable.-electrode arc melting as a production technology is growing. One advantageous feature of this process is that it avoids ingot contamination by soluble crucible materials by employing a chilled metal crucible. Because the thermal balance under these conditions is rather delicate and does not necessarily provide a favorable environment for solidification, catastrophic imbalances can occur. The effectiveness and mechanistic roles of various factors are mostly unknown, and more intelligent insight regarding the distribution of temperature and heat is needed. Experience has provided several pertinent observations, some of which are quite superficial. The most meaningful data have resulted from studies of molten pool shapes and sizes and from measurements of heat flow through crucible walls. Overall experience, intuitively interpreted and supplemented, is sufficient nevertheless as a basis for a boundary-value treatment of the problem. A mathematical analysis based on a separation of variables, using conventional differential equation methods, provides a useful solution. For a cylindrical ingot, the temperature varies as a Bessel function of an argument proportional to the radius and as an exponential function of longitudinal position. Trial calculations using the problem solution seem to verify the general correctness of the result as compared with experience. The role and nature of solution parameters are also clarified, though not entirely resolved. It is revealed that the barrier to heat flow at the ingot-crucible surface has a prominent influence. Utility of the model embodied in the problem solution is readily demonstrated by considering a variety of contemporary questions about arc melting, and it is hoped that utility can be enhanced by improvement of the model.

Jan 1, 1968

By M. S. Burton, J. E. Ritter

The sessile-drop technique was employed to study the effect of atmosphere and alloy additions of titanium and chromium on the surface tension and contact angle of nickel on sapphire substrates at 1500oC. Shear tests were conducted on the solidified sessile drops. The liquid-gas surface tension of pure nickel on sapphire was found to be 1747 ergs per sq cm, with a contact angle of 109.6 deg. The surface tension and contact angle were not affected significantly by the four atmospheres, vacuum, impure argon, pure argon, and pure hydrogen. Small additions of titanium and chromium decreased the contact angle and for the same alloy content, contact angles were lower in pure argon than in pure hydrogen. On the basis of shear-test results , the most probable cause for adhesion in the Ni-Al2O system is the formation of NiO:Al2O3 spinel at the interface; in the titanium alloy-Al2O3 system adhesion is thought to be due to a mechanical interlocking effect; in the chromium alloy-Al2O3 system adhesion is believed to be the result of solid-solution formation involving Cr2O3 and Al2O3 at the interface. In the last few years there has been considerable interest in reinforcing metals with ceramic whiskers. It has been postulated that, by reinforcing nickel with sapphire whiskers, high-temperature strengths su- perior to those of the best current nickel alloys can be achieved.&apos; To fabricate a whisker-metal composite having optimum density and strength, understanding of wettability and adherence in the system is of prime importance. Although there has been some previous research in this a a need for further studies has been cited4-8 to understand better the effects of impurities, alloys additions, and atmosphere on the wetting and bonding of metals to metal oxides. The purpose of this research was to investigate the factors involved in the wetting and adherence of nickel/nickel alloys to sapphire (single-crystal a Al2O3). Sessile-drop experiments were conducted in vacuum, impure argon, pure argon, and pure hydrogen, to determine the effect of atmosphere on the contact angle of the metals on sapphire, and the liquid-gas surface tension of pure nickel. The solidified sessile drops were sheared from the sapphire substrate to measure the bond strength between the metal and ceramic. The alloy additions chosen were titanium and chromium since both enhance the wetting of nickel on sapphire.2, 3c Also, titanium is commonly used when brazing metal-to-ceramic seals to improve adherence. Since chromium forms an oxide that is completely soluble in sapphire, it was thought that the oxide could serve as a transition phase to promote bonding between the Ni-Cr alloy and sapphire. I) EXPERIMENTAL APPARATUS AND PROCEDURE The sessile-drop apparatus was a horizontal furnace, with an induction-heated, cylindrical molybdenum susceptor in a water-cooled Pyrex chamber. This apparatus was patterned after that of Williams and Nielsen.7 A flat Pyrex window at each end of the furnace allowed temperature measurements to be made at one

Jan 1, 1968