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By Nicholas J. Grant, Michio Yamazaki

Cast copper alloys containing 10, 20, and 30 pct Ni and 0.75 to 0.80 pct Al were machine-milled into chips, then comminuted in a rod mill to fine flake powder utilizing a number of processing variables. The powders here internally oxidized, mostly at 800°C, in a low-pressure oxygen atmosphere. The consolidated powders were hot-extruded into bar stock. Room-tenmperature tension tests, stress-rupture tests mostly at 650°C, but also at 450° and 850°C, and hardness measurements after various annealing temperature treatments to study alloy stability were perfomted. Excellent room-temperature strength, high rupture strength at 650°C, and resistance to recrystallization at 1050°C were obtained. Problems in optimizing conditions for internal oxidation of Cu-Ni base alloys are discussed. THE interesting high-temperature properties of SAP' have stimulated considerable effort in the study of more refractory alloy systems where the potential for high-strength alloys at high temperature is great.2-13 A number of methods have been utilized to produce the desired fine, hard particle dispersions, of which internal oxidation2,9,7 of dilute solid-solution systems offers considerable promise by virtue of the potential for producing ultrafine, well-dispersed oxides. While most of the published works are concerned with pure metal matrices, a number of investigators have studied the effects of solid-solution strengthening.10,19 Use of more complex alloy matrices (for example, aging systems) has been unsuccessful because overaging still occurs at high temperatures in the oxide-containing alloys.14.15 Solid-solution strengthening is, however, effective at very high temperatures9,10 and might be expected to contribute importantly to the strength of oxide-dispersion strengthened alloys. For this study, internal oxidation of solid-solution alloys of copper and nickel, containing small amounts of aluminum, was chosen as the method of alloy preparation. PREPARATION OF ALLOYS Three copper alloys containing about 10, 20, and 30 pct Ni and each containing 0.75 to 0.80 pct A1 (enough to yield about 3.5 vol pct alumina) were prepared as air-cast ingots measuring 2.5 in. diameter by 6 in. high (see Table I for the analyses). Processing steps for all the alloys were as follows (also see Table 11): 1) Homogenization of the ingot at 982°C (1800°F) for 45 hr in an argon atmosphere. 2) Machine milling of ingots into fine chips. Average thickness was about 0.1 to 0.2 mm. 3) Hydrogen reduction of chips at 593°C (1100° F) for 1 hr to reduce copper and nickel oxides. 4) Rod milling of chips to finer powders. 5) Hydrogen treatment of powders as in step 3. 6) Internal oxidation of the powders. 7) Hydrogen treatment of oxidized powders as in step 3. 8) Hydrostatic compression of evacuated powders. 9) Sintering of compacts in hydrogen. 10) Hot extrusion. Variations in processing among the alloys were made in steps 4, 5, and 10 (see Table 11). In the past, two methods were utilized to internally oxidize alloy powders. Preston and Grant3 surface-oxidized dilute Cu-Al powders to obtain the necessary amount of oxygen to oxidize the solute metal (aluminum and silicon), and then permitted the formed copper oxide to diffuse and react with the solute in an argon atmosphere. Bonis and Grant4 exposed Ni-A1 and other nickel alloys to an oxygen pressure derived from the decomposition of nickel oxide at a preselected temperature, in an argon atmosphere. Both methods are applicable and can be modified to generate a range of oxygen pressures for oxidation of the solute but not the solvent metals. Procedure I: Surface Oxidation of Alloy A3, Cu-10Ni-0.76A1. Powders of -20 to +28 mesh were surface-oxidized at 500°C (932°F) to obtain the desired amount of oxygen for oxidation of the aluminum to alumina; the powder was then sealed in Vycor and heated at 900°C (1652°F) for various times up to

Jan 1, 1965

By Joseph Javes Aramburú

El presente texto describe la optimización del circuito de molienda y clasificación de la planta de hierro, el cual comprende un molino de barras y de bolas. El proceso se inicia con la exploración geológica, se determinan las reservas probadas y probables, y se establece la forma de explotarloLa eficiencia de la molienda está en función del volumen útil del molino a diferentes volúmenes de llenado que permite determinar los parámetros óptimos de la operación.

Apr 1, 2013

By W. V. Vietti, W. A. Oberlin

Crude petroleum produced in the Texas Panhandle oil field is both an asphalt and a paraffin-base oil and is further characterized by being a high-gravity crude with an extremely high cold test,. An eight-well composite of Panhandle crude showed the following characteristics: Gravity, 36.6° A. P. I. Viscosity: 61 sec. Saybolt at 100° F. 170 sec. Saybolt at 75° F. 1560 sec. Saybolt at 50° F. (stirring) Cold Test, 60° F. Distillation Test: Per Cent. Per Cent. Gasoline........................ 28.8 Wax........................... 19.2 Kerosene........................ 4.8 Asphalt........................ 13 .0 Gas oil......................... 30.7 Sulfur1......................... 0.8 Fuel oil......................... 34.7 Subsurface Conditions The original pressure in the formation in the Panhandle field closely approximated 420 Ib. gage or 435 Ib. absolute pressure. Temperatures taken indicate that the formation temperatures do not exceed 90° F. The temperatures in Table I are typical measurements taken on one lease. * A contribrition from the research department of the Marland Refining Co. of Oklahoma and the production engineering department of the Marland Oil Co. of Texas. 1 Smith [Analysis of Panhandle and Rig Lake Crudes. U. S. Bur. Mines, Circular No. 6014 (December, 1926)] found an average sulfur content of 0.6 per cent.

Jan 1, 1928

By Andrew Case

The Port Nickel facility in Braithwaite, Louisiana, is known for pioneering hydrometallurgical processes for the 'separation and recovery of nickel, cobalt and copper. Ten years ago, in 1985, a new CRI-MET process for the recovery of molybdenum, vanadium, nickel, cobalt and alumina from spent catalysts was developed and implemented. Spent- catalysts from the petroleum industry consietute the majority of feed. These are not only a valuable-source of metals, but due to EPA regulations are frequently classified as hazardous under RCRA. Molybdenum and vanadium are selectively leached in an oxidative hydrothermal step. Alumina is then extracted in a caustic digestive leach. The unique technology produces four primary commercial products l molybdenum trioxide, vanadium oxide, aluminum trihydrate and nickel-cobalt concentrate. This paper discusses the process, modifications. during ten years of operation, and the relationship of these modifications to the future of the catalyst recycling business.

Jan 1, 1995

By Robert E. Moore

Synthetic spinel is proving to be a highly effective refractory for specific applications, but its cost limits applications. Formation of spinel from a raw material such as diaspore or bauxite could provide a simple and less costly starting material. In the study reported here, finely ground (-325 mesh) diaspore from Missouri and bauxite from Guyana and China are combined with hard burned MgO (-325 mesh) in appropriate proportions to yield spinel and spinel with secondary phases. A classical sintering and dilatometer study was completed, followed by a microstructure study to determine completeness of the reactions and morphologies of the reaction products.

Jan 1, 1993

By Thomas A. Gwynn

When Lewis and Clark first pushed their boats up the Missouri River, Meriwether Lewis reported the presence of coal in the western states by saying in 1802 that it "burnt tolerably well and afforded but little flame or smoke but produced a hot and lasting fire". Lewis would have been amazed and bewildered at the history of coal development in this region and the more recent political-socio-economic-environmental confrontations of today. Certainly without this coal the railroads would not have readily pushed into our western states, and the progress of this region would have suffered. The coal industry has passed from a period when "coal was king" to a period of depression in the industry, but its importance is being revived. A contributing and simultaneous environmental concern has emerged in the nation and in many states during the past ten years, partly caused by newly imposed standards for sulfur content of fuels. Much of the midwest and eastern coal cannot be used because of high sulfur content, shifting attention to the low sulfur coal deposits of the western states. In the western states, lands disturbed by strip mining or even underlain by strippable coal are small compared to the total acreage, and usually mining operations are on lands not under cultivation. There are some farm lands being disturbed by surface mining, but this is often over-emphasized. In states like New Mexico and Arizona the percentage is less. The value of the minerals underlying the surface certainly must be considered along with the value of the surface, and sometimes proper reclamation following mining can result in higher ultimate usage of the land.

Jan 1, 1974

By Thiago de Souza Amaral

Os aços de alta resistência microligados ao nióbio tem se demonstrado uma solução ótima na fabricação de aços para utilização em perfis estruturais utilizando os conceitos já desenvolvidos para a indústria de gás e óleo. O nióbio com seu efeito refinador de grãos, com redução da temperatura de transformação entre austenitaferrita, endurecimento por precipitação e retardamento da recristalização da austenita, usado em equilíbrio com titânio, manganês e silício e os novos processos de produção com resfriamento controlado torna possível a obtenção de aços com microestrutura bainítica, baixo carbono e alta resistência mecânica. Este trabalho demonstra os pontos de destaque referentes ao projeto de estruturas utilizando estes aços, bem como uma avaliação quanto ao processo de soldagem durante a fabricação das mesmas. É possível evidenciar que a estrutura final se torna ideal para aplicação em diversos ambientes devido a sua baixa temperatura de transição dúctil-frágil, produção de uma estrutura com cerca de 10% a menos em peso, 5% a menos em custo e com excelente soldabilidade.

Aug 17, 2017

By Richard B. Diver, Mark D. Allendorf, Daniel E. Dedrick, James E. Miller, Roy E. Hogan, Andrea Ambrosini, Eric N. Coker, Anthony H. McDaniel, Nathan P. Siegel, Gary L. Kellogg

"Converting carbon dioxide and water to hydrocarbons is an attractive option for storing solar energy and, coupled with appropriate CO2 capture technology, for recycling carbon and impacting atmospheric CO2 concentrations. For any process, high solar-to-fuel efficiency is necessary for large scale viability and favorable economics. Thermochemical approaches for solar-to-fuel conversion are potentially highly efficient as they avoid the inherent limitations of photosynthesis and also sidestep the solar-to-electric conversion necessary to drive electrolytic reactions. Solar-driven two-step metal-oxide-based thermochemical cycles for producing the components of syngas, CO and H2, from CO2 and H2O are the basis of the “Sunshine to Petrol” project. Multi-cycle production of both H2 and CO has been demonstrated over several iron- and cerium-based compositions fabricated into monolithic pieces both in the laboratory and at the National Solar Thermal Test Facility. These compositions are being developed for deployment in a unique and continuous solar-driven reactor prototype, the counter-rotating-ring receiver reactor recuperator or CR5.IntroductionThe interconnected challenges posed by increasing global competition for petroleum and the increasing concentration of atmospheric carbon dioxide are now widely recognized. Meeting these challenges requires recognition that although hydrocarbon fuels are ideal energy carriers, they can no longer be thought of as primary energy sources. It is necessary to take the realistic view that our conventional fossil fuels are in fact “stored sunlight” in the form of “sequestered carbon.” This view leads to a search for options to use and store sunlight more directly.Sunshine to PetrolIn combusting hydrocarbons we unlock the energy for utilization, but we also release the carbon to the atmosphere. However, nature teaches us that with an appropriate persistent energy source, e.g. solar irradiation, it is possible to effectively reverse the combustion process and “reenergize” CO2 and H2O back into hydrocarbon form."

Jan 1, 2010

By William B. Plank

NEVER before have so many men chosen the mineral technology field for their college training. In the college year 1936-'37, 7190 such students were enrolled in the 53 schools of the United States. My last study of the mineral technology schools of the United States and Canada was made for the year -1934-'35, and the current study, as the previous one was made for the A.I.M.E. under the auspices of the Division of Mineral Industry Education. Altogether, four studies of enrollment have been made. The first three were for successive college years beginning with 1932-'33. This present one covers a two-year period, for the purpose of these studies may he served satisfactorily if they are made biannually. The data on the schools were collected in the same way as for former studies, 'namely, by questionnaire, dated in this case Nov. 18, 1936. The figures reported are therefore comparable with those of former cars.

Jan 1, 1937

By McHenry Mosier

This progress report on a national survey of the use of detachable bits in metal mines covers 10 mines. It presents comparative costs for drilling with conventional and detachable bits, describes the reconditioning of drill steel, and gives various data on rock drilling at these particular mines. Reports to follow will include similar data on drilling at other metal mines in the United States. ACKNOWLEDGMENTS This report is based on costs and data developed and furnished by the operators of the mines visited. The author is greatly indebted to the officials and staff members at these mines for their cooperation and assistance.

Jan 1, 1936

By Richard Hamburger

Calculating machines permit the use of the more rapid cotangent and semigraphic solutions of plane triangulation. The results of these methods are as accurate as those of other methods. Simple adjustment of the net, and ease of calculation encourage more complete field work. Errors in field work or in computation are easily localized.

Jan 1, 1950

By Ximing Yuan, Yongsheng Xu, Hongjie Li

A study of a static demolition agent that can be used underwater has been carried out. A new type of granulated static demolition agent with rapid reaction has been tested in several hundred experiments. It can be used conveniently and simply in the field. It demonstrates a fast reaction rate with high expansion pressures. The important characteristic of the new type of granulated static demolition agent is the ability to function underwater. It will destroy rock and the other brittle material without flyrock, vibration, shock wave, toxic gas or noise. The reaction rate can be controlled within 30-60 minutes. It is difficult to use these products when the reaction rate is less than 30 minutes and it is less efficient when the reaction rate is longer than 60 minutes. The reaction rate is slightly increased after the material is kept in storage for two years. A new type of the hydraulic device that is used to measure the expansion pressure of solid materials has been designed. The expansion pressure of the granulated static demolition agent has been tested with the device. It is shows that the expansion pressure of the granulated static demolition agent can get to 80~120MPa in 60 minutes. Also included is a discussion of the thermodynamics of the static demolition agent.

Jan 1, 2003

By P. K. Kankar, Manoj Khandelwal, Ramesht Shukla

One of the utmost severe mining catastrophes in underground hard rock mines is rock burst phenomena. It can lead to damage to mine openings and equipment as well as trigger accidents or even threat to life as well. Due to this, a number of researchers are forced to study some easy-to-use alternative methods to predict the rock burst occurrence. Nevertheless, due to the extremely multifaceted relation between mechanical, geological and geometric factors of the mines, the conventional prediction methods are not able to produce accurate results. With the expansion of machine learning methods, a revolution in the rock burst occurrence has become imaginable. In present study, three machine learning methods, namely XGBoost, decision tree and support vector machine, are utilized to predict the occurrence of rock burst in various underground projects. A total of 134 rock burst events were gathered together from various published literatures comprising maximum tangential stress (MTS), elastic energy index (EEI), uniaxial compressive strength and uniaxial tensile stress (UTS) that have been used to develop various machine learning models. The performance of machine learning methods is evaluated based on the accuracy, sensitivity and specificity of the rock burst prediction.

Mar 17, 2021

By Altemar Dettogne do Nascimento

A Máquina de Lingotamento Contínuo nº 1 da ArcelorMittal Tubarão (AMT), com capacidade nominal de 1,8 milhões de toneladas/ano, teve seu start up em 1995. A máquina é curva com raio de 10,5 m. São produzidas placas de 200, 225 e 250 mm, largura de 800 a 1650 mm e velocidade até 1,7 m/min. Em Abril de 2012, a Máquina parou para uma reforma geral. A empresa Italiana Danieli Davy Distington foi contratada para fornecer a engenharia, fabricação e entrega dos equipamentos no período de 12 meses. No ano anterior à parada da máquina, foi realizado um site survey, o que possibilitou a elaboração de um planejamento detalhado de todas as atividades. A reforma da máquina teve como objetivos principais: correção do alinhamento da máquina, substituição de estruturas oxidadas, implantação de novas tecnologias e redução do tempo de exposição dos operadores a ambientes agressivos (alta temperatura, projeção de aço, queda de cascão da panela e material particulado) através da implantação da sala remota de controle dos veios. A máquina foi colocada em operação em 10 de agosto 2012 após ter completado, sem desvios, as fases de instalação e testes. Este trabalho mostra as fases de desenvolvimento deste projeto, os resultados das tecnologias implantadas e os testes de performance para diferentes famílias de aço.

Jul 29, 2018

By Bever M. B., Floe Carl F., Hung Liang

Data on the solubility of hydrogen in iron-silicon alloys are of practical interest, as hydrogen causes gas unsoundness and embrittlement in iron and steel and is also a factor in the metallurgy of cast iron. Zapffe and Simsl have recently demonstrated that in deoxidized iron and steel castings gassiness and bleeding are primarily functions of the hydrogen content of the liquid metal. These authors also suggested convincingly that ordinary melting and casting practice provides several sources of hydrogen for absorption by the metal. Norbury and Morgan2 and Boyles3 have shown that dissolved hydrogen affects the graphitization of cast iron. Schneble and Chipman4 included in a study of the effects of superheating on the properties of cast iron an investigation of the part played by hydrogen. Schwartz, Guiler and Barnett5 investigated the significance of hydrogen in the metallurgy of malleable cast iron. A complete interpretation of investigations of this kind calls for equilibrium values of the solubility of hydrogen in the liquid and solid phases. From the theoretical standpoint, the solubility of gases, especially hydrogen, may reveal some aspects of the nature of liquid metallic solutions. This was implied in the early work of Sieverts6 on the effect of alloying additions on the solubility of hydrogen in copper. Recent work by Bever and Floe7 has shown that in liquid copper-tin alloys the solubility of hydrogen changes abruptly at the composition of the intermetallic compound Cu3Sn. It is of considerable interest to determine whether liquid alloys of iron also have compositions at which the solubility of hydrogen exhibits a discontinuous or otherwise unique behavior. Among the various alloys of iron the iron-silicon system is important because of the presence of silicon in various structural alloy steels, transformer sheets, cast irons and special acid-resisting castings. The various grades of ferrosilicon, finally, cover almost the entire remainder of the composition range. Published information on the solubility of hydrogen in iron-silicon alloys is meager. The first values for pure liquid iron were reported in 1910-191 1 sieverts and Krumbhaar8 and by sieverts.9 They found that 100 grams of iron absorbs 28 c.c. of hydrogen at 1550°C and One atmosphere pressure, and 31 C.C. at 1650°C. In 1938 Sieverts, Zapf and Moritz10 published a value of 26.3 C.C. at 1550°C. Data on the solubility of hydrogen in liquid iron-silicon alloys and in liquid silicon are not available. Martin1' investigated

Jan 1, 1947

By Bever M. B., Floe Carl F., Hung Liang

Data on the solubility of hydrogen in iron-silicon alloys are of practical interest, as hydrogen causes gas unsoundness and embrittlement in iron and steel and is also a factor in the metallurgy of cast iron. Zapffe and Simsl have recently demonstrated that in deoxidized iron and steel castings gassiness and bleeding are primarily functions of the hydrogen content of the liquid metal. These authors also suggested convincingly that ordinary melting and casting practice provides several sources of hydrogen for absorption by the metal. Norbury and Morgan2 and Boyles3 have shown that dissolved hydrogen affects the graphitization of cast iron. Schneble and Chipman4 included in a study of the effects of superheating on the properties of cast iron an investigation of the part played by hydrogen. Schwartz, Guiler and Barnett5 investigated the significance of hydrogen in the metallurgy of malleable cast iron. A complete interpretation of investigations of this kind calls for equilibrium values of the solubility of hydrogen in the liquid and solid phases. From the theoretical standpoint, the solubility of gases, especially hydrogen, may reveal some aspects of the nature of liquid metallic solutions. This was implied in the early work of Sieverts6 on the effect of alloying additions on the solubility of hydrogen in copper. Recent work by Bever and Floe7 has shown that in liquid copper-tin alloys the solubility of hydrogen changes abruptly at the composition of the intermetallic compound Cu3Sn. It is of considerable interest to determine whether liquid alloys of iron also have compositions at which the solubility of hydrogen exhibits a discontinuous or otherwise unique behavior. Among the various alloys of iron the iron-silicon system is important because of the presence of silicon in various structural alloy steels, transformer sheets, cast irons and special acid-resisting castings. The various grades of ferrosilicon, finally, cover almost the entire remainder of the composition range. Published information on the solubility of hydrogen in iron-silicon alloys is meager. The first values for pure liquid iron were reported in 1910-191 1 sieverts and Krumbhaar8 and by sieverts.9 They found that 100 grams of iron absorbs 28 c.c. of hydrogen at 1550°C and One atmosphere pressure, and 31 C.C. at 1650°C. In 1938 Sieverts, Zapf and Moritz10 published a value of 26.3 C.C. at 1550°C. Data on the solubility of hydrogen in liquid iron-silicon alloys and in liquid silicon are not available. Martin1' investigated

Jan 1, 1947

By Harold Margolin, W. R. Hibbard, R. W. Fenn, H. P. Moore

Deformation lines, also called etch markings or strain markings, are non-effaceable lines developed in individual grains by etching a metal specimen which has been cold worked sufficiently to cause atomic non-conformity or slight orientation differences within the grains. Etching occurs more rapidly at these lines of high chemical reactivity to produce a result similar to that revealing grain boundaries. Wider etching effects forming bands have been found. They are believed to be bands of deformation lines which form areas of measurably different orientation from the crystal matrix. The crystallite rotations causing these bands have been shown by Barrett2 to contribute to deformation textures. Although deformation lines have been observed in many metals, the amount of deformation requireti for their appearance has been established only in general terms. Mathewson and Phillips3 observed the first appearance of deformation lines in cold-rolled alpha brass at about 20 pct reduction in thickness using the standard ammonium hydroxide hydrogen peroxide etchant. Price and Davidson4 noted defor- mation lines in common high brass after 26.5 pct reduction by cold rolling using the same etchant. Johnson6 observed dark thick forklike lines in 99.99 pct pure copper reduced 31.8 pct. Adcock6 observed deformation lines in 80-20 copper-nickel alloy rolled 50 pct. Samans7 found no deformation lines in alpha brass single crystals cold rolled 9.5 pct but they did appear after 25 pct reduction using ammonium hydroxide and hydrogen peroxide etchant. Barrett and Levenson8 observed deformation bands in drawn polycrystalline iron at very small reductions in area and noted that their initial appearance perhaps depends on grain size and other conditions. They reported deformation bands in a single crystal of iron reduced 6 pct by drawing. Brickg noted that deformation lines in 70-30 brass apparently associated with I I I I ) planes appeared after reductions of from 20-50 pct by cold rolling. Brick and Williamson10 noted that in single crystals of 70-30 alpha brass "as in polycrystalline brass, no deformation markings appeared until reductions exceeded 20 pct." Cook and Richards" reported that in Copper cold rolled less than about 50 Pet few strain markings were apparent but for higher reductions many strain markings appeared transverse to the rolled direction. In a review article Brick and Phillips12 noted that previous studies had not shown deformation lines in cold rolled alpha brass below 20 pet reduction and added that 4

Jan 1, 1949

By H. P. Moore, R. W. Fenn, Harold Margolin, W. R. Hibbard

Deformation lines, also called etch markings or strain markings, are non-effaceable lines developed in individual grains by etching a metal specimen which has been cold worked sufficiently to cause atomic non-conformity or slight orientation differences within the grains. Etching occurs more rapidly at these lines of high chemical reactivity to produce a result similar to that revealing grain boundaries. Wider etching effects forming bands have been found. They are believed to be bands of deformation lines which form areas of measurably different orientation from the crystal matrix. The crystallite rotations causing these bands have been shown by Barrett2 to contribute to deformation textures. Although deformation lines have been observed in many metals, the amount of deformation requireti for their appearance has been established only in general terms. Mathewson and Phillips3 observed the first appearance of deformation lines in cold-rolled alpha brass at about 20 pct reduction in thickness using the standard ammonium hydroxide hydrogen peroxide etchant. Price and Davidson4 noted defor- mation lines in common high brass after 26.5 pct reduction by cold rolling using the same etchant. Johnson6 observed dark thick forklike lines in 99.99 pct pure copper reduced 31.8 pct. Adcock6 observed deformation lines in 80-20 copper-nickel alloy rolled 50 pct. Samans7 found no deformation lines in alpha brass single crystals cold rolled 9.5 pct but they did appear after 25 pct reduction using ammonium hydroxide and hydrogen peroxide etchant. Barrett and Levenson8 observed deformation bands in drawn polycrystalline iron at very small reductions in area and noted that their initial appearance perhaps depends on grain size and other conditions. They reported deformation bands in a single crystal of iron reduced 6 pct by drawing. Brickg noted that deformation lines in 70-30 brass apparently associated with I I I I ) planes appeared after reductions of from 20-50 pct by cold rolling. Brick and Williamson10 noted that in single crystals of 70-30 alpha brass "as in polycrystalline brass, no deformation markings appeared until reductions exceeded 20 pct." Cook and Richards" reported that in Copper cold rolled less than about 50 Pet few strain markings were apparent but for higher reductions many strain markings appeared transverse to the rolled direction. In a review article Brick and Phillips12 noted that previous studies had not shown deformation lines in cold rolled alpha brass below 20 pet reduction and added that 4

Jan 1, 1949

By J. Brett, L. Seigle, L. Castleman, T. Montelbano

Impurity-induced low-temperature recrystallization of cold-worked tungsten was inuestigated with emphasis on the influence of nickel on the reaction. Palladium, nickel, aluminum, manganese, platinum, and iron greatly lower the recrystallization temperature of doped tungsten, which zs normally very high, but the recrystallization temperature of electron-be am zone-refined tungsten wzre is slightly raised by conlacl with nickel. Recrystallization can be induced at low temperature by the presence of solid nickel on the surface of doped tungsten wire, but apparently not by exposure to nickel vapors alone. Approximately 200 ppm of Ni dijjused into 10-mil wires at 1200 from a deposit of nickel on the surface produced total recrystallization, whereas more than 600 ppm of Ni could be absorbed frotn a vapor source without altering the fibrous structure of cold-worked tungsten. Once initiated, nickel-induced recrystallization required a continued source of' nickel for propagation of the recrystallization front. The solubility of nickel in fibrous 10-mil W wire was approximalely 500 ppm at 1150' C, and the activation energy for penetration of the recrystallization front was 52 kcal per mole. In many applications the usefulness of tungsten depends on critical control of its structure. Cold-worked tungsten with the fibrous structure developed by suitable thermo-mechanical treatment has a low, but technologically significant, ductility. It has long been known1 that traces of nickel, and perhaps other metals, are profoundly deleterious in doped tungsten, because they induce recrystallization at low temperature, which produces a brittle, equiaxed grain structure. This effect appears to be an exception to the general observation that recrystallization is impeded and the recrystallization temperature raised by the presence of impurities.2"9 Previous studies7-'' of the annealing and recrystallization of tungsten wire have divided the phenomenon into prior recovery stages, primary recrystallization and secondary recrystallization. The present investigation is concerned principally with primary recrystallization which is defined here as the replacement of the fibrous structure of deformed tungsten by equiaxed grains. The objective of this study was to explore the nickel-induced recrystallization reaction in tungsten and attempt to elucidate its mechanism. As well, an effort to define which other elements give rise to low-temperature-induced recrystallization was carried out. EXPERIMENTAL PROCEDURE The procedure adopted for these experiments was essentially to bring nickel and other elements into diffusive contact with cold-worked tungsten wires. The process of recrystallization was followed as a function of time and temperature by light and electron microscopic observations. First the influence of nickel on the recrystallization temperature of arc-melted, zone-refined, and variously doped tungsten wire was determined by electroplating a deposit of nickel on the surface of the wire and annealing at a variety of temperatures for 3 hr. The chemical analyses of the tungsten wires used in this investigation are given in Table I. The surface of the tungsten wire was etched with Murakami's slution' and approximately 0.005 in, of Ni was deposited from a Watts-type low pH bath14 for the conditions of these experiments. Variations in plating thickness from about 0.001 to 0.005 in. had no discernible influence on the resulting structures. The wires were then annealed in an atmosphere of dry hydrogen to establish the recrystallization temperature. Concurrently, un-plated specimens were annealed to establish the recrystallization characteristics of nickel-free wire. The criterion of recrystallization was that the fibrous structure be completely replaced by equiaxed grains after a 3-hr treatment of temperature. This provided more reproducible results than use of the first recrystallized grain or a fixed proportion of re-crystallized structure as the critical observation. The structures encountered in longitudinal and transverse sections were examined by both light and electron microscopy at magnifications up to X32,000 using parlo-dion-carbon replicas shadowed with platinum for the latter method. Second, the influence of a variety of metals on the recrystallization temperature of 0.010 in. D alumina-silica doped tungsten wire, AW136-64, was determined. The elements were applied by electroplating whenever possible. Alternatively, they were vapor-plated on the tungsten wire and a greater thickness built up by coating with a dispersion of metal powder in nitrocellulose lacquer. Elements not amenable to either of these procedures were merely slurry coated on the tungsten. The recrystallization temperature was determined as above. Third, the nickel-induced recrystallization process in doped wire was studied more closely by electroplating 8 mils of Ni on 65-mil alumina-silica doped tungsten wire, AW153-NS10, and exposing the wire to temperatures of llOO°, 1200°, or 1300°C for various times in a hydrogen atmosphere. A circular recrystallization front, 'Onsisting of equiaxed grains, developed at the periphery Of the coated tungsten wire, and the advance of this front into the fibrous interior was studied. These experiments employed relatively coarse 0.065 in. D wire because the 0.010 in. D wire recrystallized too quickly to permit observation of the pene-

Jan 1, 1969

By Edward Judd

CANADA'S mining industry is rapidly recovering from the depression through which it passed in 1921. Its total output of $183,029,600 in 1922 was 6.4 per cent. greater than that of 1921, and was exceeded by only three previous years, 1917, 1918, and 1920. Table 1 compares the output of a few of 'the more important items selected from preliminary data published' by the Dominion Bureau of Statistics. TABLE 1.-OUTPUT OF CERTAIN MINERAL PRODUCTS IN CANADA PER CENT. 1921 1922 CHANGE Cobalt, metal and in compounds, lb 252,000 443,800 +76.1; Copper contents of blister, matte, and exported ores, lb 47,620,820 43,321,400 - 9.0 Refined copper, lb 4,286,000 730,000 -83.0 Gold, fine oz 926,329 1,230,985 +32.8 Pig iron, sh. tons 665,676 429,024 -35.5 Lead, sh. tons 33,340 47,085 +41.2 Nickel contents of matte, etc., lb. 19,293,060 17,496,490 - 9.3 Silver, including that in base bullion, gold bullion, etc., fine, oz. 13,543,198 17,611,646 +30.0 Zinc (nearly all refined), sh. tons. 26,545 28,199 + 6.2 Asbestos shipments, sh. tons 92,761 136,657 +47.3 Coal, all grades, sh. tons 15,057,500 15,045,300 Gypsum shipments, sh. tons 386,550 441,160 +14.1 Natural gas, M. cu. ft 14,077,600 14,954,100 + 6.2 Petroleum, bbl : 187,540 178,570 - 4.8 Cement, bbl 5,752,885 6,943,968 +21.0 Brick, structural, all kinds, M. , , 109,009 127,137 +17.0 On the basis of estimated market values, the whole output of 1922 was contributed as follows: Metals, 33.4 per cent.; non-metallic minerals, 45.1 per cent.; structural materials and clay products, 21.5 percent.; this distribution indicates a return of the metal mining. industry nearly to the position of relative importance that it occupied. before 1921, in which year metals contributed only 28.7 per cent. to the total value. of output while non-metallics gave 51.1 per cent. Canadian cobalt originates entirely in the ores of the Cobalt district, which are mainly treated at smelters in southern Ontario, although some quantities of residues have been exported to England and Europe. Exports during 1922 increased even more than production, consisting of about four-fifths . cobalt oxides and salts, and one-fifth of cobalt alloys and other metal combinations.

Jan 8, 1923