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By William J. Campbell

One of the principal objectives of the Bureau of Mines program for developing super refractory materials is to obtain fundamental data on the physical properties of refractory oxides. This particular investigation obtained accurate thermal expansion coefficients for alpha alumina and evaluated, critically, those coefficients with other published values. High-temperature X-ray diffractometer measurements, by the Bureau, showed that alpha alumina expands anisotropically with expansion parallel to the c axis approximately 10 percent greater than parallel to the a axis. Thermal expansion characteristics of four different alumina samples were determined up to 1,200° C.; the results are presented in both tabular and graphical form. The combined random and systematic errors in the measurements are considered less than 3 percent above 500° C, and approximately 2 percent at 1,000° C. No differences in expansion were observed between the samples or between the heating or cooling cycles.

Jan 1, 1961

By D. H. Baker

These investigations were conducted to determine the feasibility of molten salt electrorefining of zirconium scrap, offgrade sponge, and alloys under contract number AT(11-1)-475 between the Atomic Energy Commission and the Federal Bureau of Mines. Offgrade zirconium sponge having a Brinell hardness of 169 can be refined by this technique to produce metal having, consistently, a Brinell hardness of less than 90. Also, zirconium alloy scrap, approximating zircaloy-2 in composition, can be refined to recover zirconium metal with a Brinell hardness of less than 100 that is essentially free of the major alloying elements. Analysis showed that the quantities of these elements were decreased as follows: iron from 0.27 to 0.002, tin from 1.36 to 0.001, nickel from 0.02 to 0.001, and chromium from 0.12 to 0.002 percent.

Jan 1, 1961

By James E. Mauser

This report deals with the investigation of a continuous process for producing pure zirconium. It covers the construction, operation, and maintenance of the semicontinuous reactor. The report covers a study of test variables, such as reactor temperature and reluctant charge weights, and evaluates the results, such as billet metal hardness, residual billet salt content, and suitability of a purified billet as a consumable electrode for arc melting. The purpose of this project was to develop an inexpensive and continuous process for producing pure zirconium. The process developed, termed the semicontinuous reactor process, produced billets of compacted zirconium sponge. The metal was produced by reducing zirconium tetrachloride with sodium and magnesium beneath molten byproduct salt. Hydraulic rams at each end of a vertical reaction tube compacted the sponge and ejected it as a billet. These billets were purified by heat under vacuum to remove entrapped salt. The goal was to utilize the purified billet directly as a consumable electrode for arc melting.

Jan 1, 1961

By R. L. Grant

The principal official test performed by the Bureau of Mines to determine the permissibility of coal-mine explosives, commonly referred to as the gallery test, has been in use at the Bruceton station for many years (2, 16).4/ In this test the explosive under study is loaded into the borehole of a steel cannon and fired into a flammable mixture of natural gas and air or natural gas, air, and coal dust. To meet the requirements for permissibility, the explosive must not ignite the gas mixture under the conditions of the test. There is little doubt that these tests have succeeded in the main objective, namely, to screen the relatively safe from the relatively hazardous explosives. It has been generally conceded that adoption of permissible explosives by the coal-mining industry in the United States has substantially reduced the frequency of disastrous underground explosions caused by blasting. In recent years, however, research workers planning programs for improving the safety of coal-mine explosives have felt the growing need of a more quantitative method for measuring the incendivity of explosives based on a better understanding of the role of the important variables in the gallery tests, Accordingly, it was decided to apply certain statistical methods and techniques to the gallery test to develop it into a more precise tool for evaluating permissible explosives. One of the first and more important methods applied for this purpose was the up-and-down technique (6,7,17), It was demonstrated (14,15) that the weight of the explosive charge directly affects the ignition probability of the natural gas-air atmosphere and that the curve of ignition probability versus charge weight is a cumulative normal curve. Following these experiments, a program, still in progress, was set up to study how the addition of sodium chloride to various permissible-type ex-plosives affects their incendivity. This program resulted in 3,294 shots,

Jan 1, 1961

By W. M. Dressel

The Federal Bureau of Mines has obtained data by differential thermal analysis of the various minerals that represent the nation's resources in manganese. These data are supported by X-ray diffraction analysis, chemical analysis, mineralography, and optical mineralogy, and provide fundamental information on the response of each mineral to thermal treatment in oxidizing, reducing, and neutral atmospheres. The information can be applied advantage¬ously in the identification of manganese minerals. Its greatest potential value, however, lies in the application of the quantitative data on the reaction temperatures, rates, and products to the more efficient extraction of manganese from U.S. ores. Thermal analysis curves are presented for certain manganese minerals, namely hausmannite, bixbyite, braunite, pyrolusite, lithiophorite, cryptomelane, hollandite, manganite, rhodochrosite, and rhodonite. The original minerals and the products of their thermal decomposition were identified by X-ray diffraction analysis, supplemented by chemical analysis and mineralogical identification.

Jan 1, 1961

By R. P. Jewett

The object of this investigation was to correlate the crushing strength of green pellets prepared from magnetite, specular and earthy hematite with the particle size of these respective raw materials. In this study no attempt was made to correlate the strength of fired pellets and particle size. The effect of particle size upon a number of fine ores and concentrates was studied. Much of the low-grade ore reserves in the Lake Superior Region must be finely ground before concentration and then agglomerated for iron and steelmaking processes. Fine natural ores also must be agglomerated. Pellets constitute an important type of agglomerate. Considerable handling occurs during screening to remove undersize and oversize pellets, and in transfering green unfired pellets from the balling machines to the heat-hardening equipment. As a result the strength of the green pellets is a factor of great importance.

Jan 1, 1961

By E. C. Perkins

The purpose of the research described in this report was to develop techniques for using ilmenite from domestic deposits for the production of titanium tetrachloride. The research was done by the Federal Bureau of Mines in cooperation with the General Services Administration under contract DMP-116, Utilization of Domestic Ilmenite. Bench-scale continuous chlorination of an Idaho ilmenite containing 27.9 percent titanium and 35.6 percent iron yielded a crude titanium tetrachloride suitable for purification and for the production of titanium metal and pigment. A summary of the results of 380 hours of operation showed that 82.4 percent of the titanium was chlorinated, with 92.5 percent utilization of chlorine. The construction- of a. quartz tube chlorinator 4-inches in diameter and 24 inches long is described with the necessary details of operation.

Jan 1, 1961

By H. S. Caldwell

The objective of this investigation by the Bureau of Mines was to develop and test for laboratory use a retort embodying many features required for practical commercial-scale applications of vacuum distillation of metals. A gas-fired vacuum retort was developed comprising a hollow, cylindrical graphite liner encased in a thin shell of stainless steel. The liner prevents the shell from collapsing under vacuum and protects it from corrosion by metal vapors and the molten metal charge. The vacuum-tight shell protects the liner from oxidation and flame erosion. The retort was used to distill zinc from dross and die-casting scrap. More than 99 percent of the zinc was recovered as a condensate containing 99.8 to 99.9 percent zinc. (Atmospheric distillation recovers 95 to 98 percent at a purity of 99.5 percent zinc.) Distillation rates of 50 pounds of zinc per hour were attained at a temperature of 65° C. with pressures ranging between 50 and 100 microns. Distillation at this low temperature is not practicable at atmospheric pressure. Also, the retort is suitable for distilling other volatile metals such as cadmium and magnesium.

Jan 1, 1961

By A. E. J. Gallagher

This report summarizes the results of flotation studies conducted by the Federal Bureau of Mines on samples of extremely fine-grained lead-zinc sulfide ores. Samples from five ore deposits in the Pine Creek area, Coeur d'Alene district, Idaho, and one deposit in the Metaline district, Washington, were studied at the Albany Metallurgy Research Center to determine the recovery of sulfide lead and zinc by flotation. During the investigation it was found that flotation could be effectively applied to the selective recovery of exceedingly fine-grained lead and zinc sulfide minerals. Separation of galena and sphalerite was obtained on pulps ground through 1,600-mesh, in which most of the particles were smaller than 5 microns. Selectivity and recovery of minerals in this fine size range were enhanced by use of a chemical dye, diphenylthiocarbazone, as a galena promoter. Although unsuccessful on one ore, application of the dye in treatment of two other very fine-grained ores yielded lead concentrates containing over 62 percent Pb at recoveries in excess of 85 percent. More than 55 percent of the lead in these concentrates occurred as particles smaller than 2 microns.

Jan 1, 1961

By Miles B. Royer

The experimental blast furnace has attracted increasing interest during the past decade as a practical means for investigating a broad range of blast-furnace smelting problems. Under experimental-furnace conditions, information can be obtained with less expenditure of time and raw materials and, therefore, at lower cost than comparable information could be obtained under industrial operating conditions. Furthermore, the experimental furnace may be operated beyond the range of smooth operation, even to failure, to delineate the limits of operability. Such deviation from normal operating practice would be economically intolerable in industrial operations where production and operating stability might be disrupted. The Federal Bureau of Mines experimental blast furnace at Bruceton, Pa., near Pittsburgh, has been operated and under development since 1951. However, the usefulness of this experimental data to industrial practice was somewhat nebulous in early experiments, and the correlation of the experimental blast furnace with the industrial blast furnace was not known.

Jan 1, 1961

By A. W. Decora

Gas-liquid chromatography has been applied to separating basic nitrogen compounds, such as pyridines and amines. Close-boiling compounds have been separated by exploiting structural and polarity differences, using selective liquid substrates dispersed on specially prepared solid supports. Development of these special supports was necessary in order to obtain symmetric peaks for basic nitrogen compounds; solution of this problem was important in applying gas-liquid chromatography to the analysis of basic nitrogen compounds found in shale oil. Attempts to analyze shale-oil tar bases by conventional gas-liquid chromatographic techniques, using Chromosorb4/ or Celite 545 as the support for a nonpolar liquid substrate, resulted in asymmetric peaks. These asymmetries were caused by adsorption of sample vapors on the solid support. Symmetric peaks were obtained when strongly polar liquid substrates were used on either Chromosorb or Celite. However, a solid support giving symmetric peaks only with strong polar substrates restricts the choice of substrate, and frequently, desired separations cannot be achieved.

Jan 1, 1961

By J. D. Ramsdell

The object of this investigation by the Federal Bureau of Mines was to evaluate the workability, recrystallization characteristics, and mechanical and physical properties of high-purity electrorefined vanadium. The low level of interstitially soluble elements in electrorefined vanadium results in a soft ductile metal which responds readily to cold working by rolling, swaging, and press-forging. Hardness, strength, and resistivity increased with an increase in impurity content, but thermal expansion was independent of impurity content. The work-hardening of vanadium occurs rapidly. Most of the hardness increase occurs in the first 15 pct. of reduction in area. When vanadium is annealed, its hardness increases to a maximum when the annealing temperature is between 200° to 400° C. A sharp decrease in hardness develops as the annealing temperature is increased. An anomaly in the hardness versus annealing temperature curve is present in the 600° to 800° C. range, while all evidence of cold-work is removed at annealing temperatures above 900° C.

Jan 1, 1961

By Perry G. Cotter

The borides of the transition metals in Groups IV and VI exhibit, in addition to a certain degree of hardness, considerable resistance to heat and oxidation. They have high melting points (1,850°-3,060° C.) and low coefftcients of thermal expansion and can be bonded with other materials and hot-pressed to desired shape (cermets). Suggested uses for the borides include use in rockets and jet engines, as thermocouple protection tubes, as containers for molten metals in die casting, as flame-plated coatings on less refractory compositions to prevent erosion by hot gases, and as control rods and neutron shielding material in nuclear engineering, The Federal Bureau of Mines investigation of zirconium diboride started in 1950 at the Boulder City Nev,, Metallurgy Research Laboratory, Its purpose was to reduce the cost of raw materials for the production of zirconium diboride.

Jan 1, 1961

By J. W. Town

As part of the Federal Bureau of Mines titanium resources examination program, samples from seven deposits in the Pacific Northwest were tested for amenability to various beneficiation techniques. The samples obtained by the Bureau's Office of Mineral Resources at Spokane, Washington represent a large potential source of titanium. This report summarizes the results of tests at the Bureau's Metallurgy Research Center, Albany, Oregon. Recoveries from tabling placer samples were about 50 percent at grades of 30 percent titanium dioxide. Flotation was the most effective method for concentrating the fine ilmenite in clay samples; recoveries of approximately 50 30 percent titanium dioxide. Flotation was the most effective method for concentrating the fine ilmenite in clay samples; recoveries of approximately 50

Jan 1, 1961

By C. N. Adams

The purpose of this investigation was to evaluate the physical and mechanical properties of high-purity titanium made by two processes. Sodium-reduced metal with 58 Brinell hardness number (B.h.n.) and electrorefined metal with 60 B.h.n. and 70 B.h.n. were used. Titanium of these hardness levels did not work-harden excessively, and beyond 40 percent cold work the hardening effect was not great. Rapid softening occurred when the metal was annealed at temperature between 300° and 600° C. Full annealing, as determined by property and microstructure studies, was accomplished after 30 minutes at 700° C. A recrystallization diagram is presented which is based on determinations of annealed grain size as a function of rolling reduction and annealing time. For reductions of less than 20 percent, exaggerated grain growth occurred during annealing; for reductions greater than 20 percent, the variation in grain size for each annealing temperature was minor.

Jan 1, 1961

By Leland A. Yerkes

Refining aluminum from crude aluminum alloys by the subhalide reaction was investigated to develop a method of producing aluminum by means other than electrolysis of its oxide. The best materials and design for the apparatus and also optimum operating conditions, including temperature, pressure, vapor flow rate, and composition of alloy charge were studied. In the subhalide process, aluminum-trihalide vapor reacts with aluminum in the alloy under high temperature and low pressure, forming volatile aluminum monohalide which reverts to aluminum metal and aluminum trihalide on cooling. The only halide used in this investigation was aluminum trichloride. The crude aluminum-silicon alloys used as the principal raw material contained from 21.9 to 36 percent aluminum, and significant quantities of iron and titanium. These alloys were produced by direct electric smelting of clays. Graphite tubing that was heated by an induction coil proved to be satisfactory material for the laboratory reactor chamber, Enclosed in an insulated glass or quartz pipe, the reactor was used in both vertical and horizontal positions with various baffle and tray arrangements for directing the trihalide vapor both over and through the alloy. Aluminum trichloride vapor was generated in the sublimer at one end of the glass pipe, passed into the reactor where contact was made with the crude alloy, and aluminum monochloride gas was formed. When the gaseous mixture of aluminum monochloride and unreacted tri-chloride passed out of the reactor and entered the condenser, the gases were cooled to 900° C. or less, causing the monochloride to disproportionate into aluminum and aluminum trichloride vapor. The aluminum was deposited on the condenser walls while the aluminum trichloride vapor was carried out of the condenser and into the opposite end of the glass pipe where it solidified on the cooled copper coils.

Jan 1, 1961

By Perry G. Cotter

The objective of this investigation was to synthesize and investigate the properties of a high-temperature refractory material based on a combination of boron, silica, and magnesium. A magnesium-thermic reaction was used for the synthesis. X-ray examination of the product indicates that the crystalline portion of the composition is a combination of magnesium borides, magnesium silicate, and magnesium orthoborate. Chemical analysis of a representative sample shows, in weight-percent, boron 17.6, silicon 23.9, magnesium 17.8, and chromium 0.5. The balance is largely oxygen. The composition is resistant to high temperatures under oxidizing conditions and is stable in water, hydrochloric acid, and hydrogen. It has a low density (less than 3 grams per cubic centimeter) and a hardness value in the range of quartz. It has a melting point above 1,700° C. and can be hot-pressed to shape in the temperature range between 1,200° and 1,350° C. The properties described in this paper indicate that the material may have some uses as a high-temperature refractory, and because of its boron content it may have some value as a thermal-neutron-absorption material.

Jan 1, 1961

By H. C. Fuller

Depletion of iron ore in the Nation's large deposits has directed attention to other sources. One of these is the titaniferous iron ore of the Iron Mountain, Wyo., area. Tests were made to determine the feasibility of smelting this ore, which contains about 20 percent titanium dioxide (Ti02), in an electric-arc furnace to produce pig iron. Initial tests, which were made in a 30-pound-capacity induction furnace, demonstrated that the iron could be easily reduced to metal and that limestone was a suitable and effective flux. Larger scale tests then were made in a 50-pound-capacity electric-arc furnace to obtain the more detailed information necessary for the planned continuous operation of a still larger arc furnace. The principal facts determined by preliminary batch-smelting studies were that (1) 9 pounds of limestone flux was required for each 100 pounds of ore smelted, (2) expensive coke was not required because coal proved to be a satisfactory reductant (near stoichiometric carbon was optimum), and (3) overreduction, which produced a viscous slag, must be avoided.

Jan 1, 1961

By Beverly W. Dunning

The effect of vacuum melting on the elimination of gases and nonmetallic inclusions for six low-alloy steels was investigated. The purpose of these studies was the analysis and comparison of differences in gas content and inclusions in air-melted and vacuum-melted steel. Data obtained from melts of 1-1/4 to 20 pounds indicate that vacuum melting decreases the number and size of nonmetallic inclusions and at the same time increases the degree of dispersion of the remaining inclusions. These improvements are undoubtedly related to the elimination of approximately 80 percent of the nitrogen and 90 percent of the oxygen as well as most of the undesirable metallic trace impurities.

Jan 1, 1961

By J. G. Walters

In 1928, the Coal Carbonization Section of the Federal Bureau of Mines, in cooperation with the American Gas Association, began a survey of the carbonizing properties of American coals. A standard test method for evaluating the carbonizing properties of coals that met the following conditions was developed: To yield products similar to those obtained in commercial operations. To produce yields sufficient to permit analyses and tests of quality. To be laboratory size. To be convenient to operate. To permit reproducible control of test conditions and results. This test method has become known as the Bureau of Mines-American Gas Association (BM-AGA) test (53),3/ and more coals of greater variety have been tested in this apparatus than in any other of similar scale.

Jan 1, 1961