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By J. H. Scaff, H. C. Theuerer

Germanium may be reversibly converted from n to p type by heat treatment. Data for the conversion and the associated changes in resistreatment.tivity are given and the results are interpreted in terms of changes in the donor-acceptor balance. MEANS for controlling the electrical properties of germanium in a predictable manner are of interest because of the increasing utilization of this element as the semiconducting material in electrical devices. Since both the mechanism and the magnitude of the electrical conductivity depend upon the kind and quantity of impurities present, the conductivity usually is adjusted by first carefully purifying the germanium, and then, by standard alloying procedures, adding the elements desired. The elements usually added are from the third or fifth periodic groups depending upon whether p- or n-type germanium is desired. However, in the development of germanium rectifiers during the war, it was found that it was possible also to modify reversibly the conductivity of germanium and even to produce conversion from n to p type by heat treatment.1,5 Since then a detailed study of this effect has been made. The data are presented in this paper and an explanation is offered for the effects observed. Preparation and Experimental Procedure The method used in preparing the germanium ingots for this investigation has been previously described.' The method consists essentially of (1) reduction of GeO2* and (2) preparation of a 50-g ingot from the reduced material. Graphite containers are used in both steps. In the first step the GeO2 is reduced in hydrogen at 650 °C to form a sponge germanium which, to assure complete reduction and to obtain massive materials, is fused subsequently in the reduction furnace by gradually raising the temperature to 1000°C. The button of germanium thus obtained corresponds to a yield of 99.8 pct. The final ingot is prepared by fusion of the germanium button in a helium atmosphere. A cylindrical crucible in a vertical silica tube furnace is employed and the crucible is heated by an external induction coil. The ingot is solidified from the bottom upward by raising the induction coil at a constant rate with power to the coil kept at a fixed value. In such ingots, segregation is normal and most of the impurities are concentrated in the last region of the ingot to freeze. It follows then that the major portion of the ingot is purer than it would have been if freezing had occurred in a random fashion. Moreover the orderly advance of the freezing surface during solidification establishes in the ingot a succession of surfaces of constant composition, if it is assumed that the liquid is homogeneous and that diffusion in the solid is negligible. Therefore, some information on the distribution of impurities in the ingot may be acquired by determining the shape of the solid-liquid interface at different stages of solidification. This is of importance because the concentration of impurities will be seen to affect the response of germanium to heat treatment. Such information is difficult to acquire by direct means, for the impurities responsible for the electrical properties of germanium prepared in this way are present

Jan 1, 1952

By A G. Dempster, N Barnett, J Oh, S Saydam

NASA’s Artemis III mission is expected to return astronauts to the surface to explore and sample the lunar volatiles by 2026. These volatiles are anticipated to provide scientific insights as to how the Moon was created and economic value to off-Earth operations. These same volatiles can pose health implications to astronauts and Earth based personnel handling lunar regolith samples. Using Australian, USA and NASA airborne contaminant exposure limits and the Lunar CRater Observation and Sensing Satellite (LCROSS) measurements of lunar volatiles in the Cabeus crater ejecta, the minimum mass of lunar regolith that can be safely handled by humans on Earth and in spacecraft can be calculated. This analysis determined a 0.15 grams pure sample of Cabeus crater regolith within a cubic metre of air has enough volatiles to exceed safe working conditions, and 14.9 grams of pure Cabeus crater regolith per cubic metre of air can impact human life. The intent of this analysis is to assist safe handling and exposure calculations for the safe handling procedures of lunar regolith containing volatiles.

Sep 1, 2024

By R Grogan

Nautilus Minerals Inc is a sea floor resource exploration and development company focused on developing the Solwara 1 Project, a copper-gold sea floor massive sulfide deposit in the territorial waters of Papua New Guinea, for which it holds a mining lease and associated environment permit.Economies depend upon four key types of capital: built, natural, financial and human. Natural capital consists of the ‘minerals, energy, plants, animals, ecosystems (climatic processes, nutrient cycles and other natural structures and systems) found on Earth that provide a flow of natural goods and services’ (Daly and Farley, 2004). Many ecosystem goods such as fish, fruit and water are already valued and sold in markets; however, some ecosystem services are not amenable to markets and have remained unvalued in traditional accounting methods, even though they provide significant value (such as flood protection, climate stability etc; Batker and Schmidt, 2015).There are now economic methods available to quantify and value natural capital and many non-market ecosystem services. When valued in dollars, these services can be incorporated into a number of economic tools, including benefit-cost analysis, accounting, environmental impact statements, asset management plans and rate of return on investment calculations. Their inclusion ultimately strengthens decision-making. When natural capital assets and ecosystem services are not considered in economic analysis, they are effectively valued at zero. This omission can lead to poor decisions, inefficient capital investments, higher incurred costs and losses due to unexpected events (Batker and Schmidt, 2015).In 2015 Earth Economics was commissioned by Nautilus Minerals Inc to conduct an independent, objective environmental and social benchmarking analysis of the proposed deep seabed Solwara 1 mine with terrestrial copper mines (referred to as ‘the report’). The report represents the first ever natural capital accounting and ecosystem goods and services framework for seabed mining.The report compares the proposed Solwara 1 mine with three terrestrial mines: Bingham Canyon (Utah, USA), Prominent Hill (South Australia, Australia), and Intag (a proposed mine in Intag Province, Ecuador), and provides a natural capital accounting assessment for all four operations.CITATION:Grogan, R, 2016. Natural capital accounting – a sea floor mining application, in Proceedings Life-of-Mine 2016 Conference, pp 2–4 (The Australasian Institute of Mining and Metallurgy: Melbourne).

Jun 28, 2016

By J. S. Ross

OIL-FIELD waters enter into many underground problems with which the petroleum engineer has to deal. Whether the problem is one of infiltration or natural encroachment, it is always desirable to determine the source of the water before commencing repair or remedial work. The usual mechanical tests for determining the source of extraneous water in wells are slow and expensive. An excellent means for the identification of oil-field waters may be afforded by their chemical characteristics when the chemical character of waters from the various sands has been established, by careful sampling and analysis cautiously interpreted. In the Salt Creek field, Wyoming, a fairly high degree of efficiency has been attained in the controlof field operations by utilizing the information afforded by the analysis. All of the operating companies appreciate this means of identifying waters, with the result that water-sampling has become general practice. Most of the chemical work dealing with Salt Creek waters has been done since the laboratories of the Midwest Refining Co. and the U. S. Geological Survey, were established in the field; the former in 1922, the latter in 1924. A spirit of cooperation has existed between the company and the government personnel by which many of the data for this paper were made available.

Jan 1, 1928

It is a common misconception that the grant of mining tenure, whether it be an Exploration Permit, Mineral Development Licence or Mining Lease, will entitle the holder to access all land within it in order to explore or mine. The ability for miners to access their tenure in order to undertake activities is critical to the industry. While significant time and energy is quite rightly dedicated to resolving native title and cultural heritage issues before the commencement of mining operations, the same cannot always be said for addressing potential impediments that arise as a result of the overlap between mining and other tenures. Miners should be aware of the overlaps that occur with other tenure and the impact of these overlaps on the minerÆs ability to explore or produce from the area. The existence of an overlap with petroleum tenure, nature refuges, national parks, wild river areas or reserves such as aboriginal land leases are all likely to have an impact on the minerÆs ability to access the area and conduct activities. In some instances, such as an overlap with petroleum tenure, Queensland legislation encourages the miner to reach agreement with the holders of the overlapping tenure. However, in other instances, such as an overlap with a national park, mining tenure is unlikely to be granted at all. This paper summarises the impacts and impediments that arise as a result of overlaps of tenure that are likely to affect mining operations. It also provides examples of how these impediments can, if possible, be overcome under Queensland legislation.

Jan 1, 2007

By Leszek Maldzinski

The present concept assumes carrying out the process of controlled nitriding with NH3 alone. This is a simpler process than that using two-component mixes of ammonia diluted with N2 or NH3diss. The regulation of the chemical composition of the atmosphere in the retort, and therefore the regulation of the nitriding potential KN, is obtained through the variation of the inflow rate of NH3 into the retort. What is a completely new things in a relevant process, the inflow of NH3 into the furnace is at times reduced to zero, which widens the range of the gas composition in the retort (and by the same token, of KN). The amount of NH3 introduced into the furnace is regulated (controlled) with the aid of a gas analyzer (for example an infrared analyzer). The gas analyzer opens and closes periodically the NH3 inlet valve with a frequency maintaining a desired gas composition (a desired KN) in the retort. The concept was based on experimental and theoretical investigations in term of thermodynamic and kinetic of gas nitriding. Investigations were carried out in a laboratory furnace with a quartz tube and also in an industrial furnace with a steel retort and a circulating fan. Nitriding was performed using NH3, NH3+H2, NH3+NH3diss. mixtures. In an industrial furnace the supply of NH3 into the retort was periodically closed, though with an operating circulation fan. The studies demonstrated that the growth rate of nitrided layer depends only on the composition of the atmosphere, (or KN), in the retort. It depends neither on a type of atmosphere introduced into furnace (NH3, NH3+NH3diss. or NH3+H2) nor a type of furnace (laboratory with a quartz tube or industrial with steel retort and fan). The results proved also that entirely closing of NH3 supply to the retort does not affect the growth rate of nitrided layer. A detailed analyses of the results was performed in a paper.

Aug 16, 2017

By A Grant, H Thomas, C Clarke, B Fuller

Native seed and plants are often a core input into the rehabilitation process of mine closure. Native plant establishment rate and performance is a function of many input elements including seed quality (purity and germination percentage), processing, treatment, storage, supply chain handling, application and ongoing management. Traditionally native seed has been supplied with very limited supporting information which in some cases has led to establishment failures, repeated attempts at successful plantings, and biosecurity issues, leading to increased rehabilitation costs for mining companies. Product procurement scrutiny, and sustainability credential requirements, in all supply chains is increasing the need for transparent, accurate, verified, and certified information. This collectively continues to evolve towards a social license to operate in all industries, including mining. The Australian Seeds Authority (ASA), in partnership with native seed supplier AustraHort, traceability software company Trust Provenance and supporting partners including Transport for NSW and Queensland Transport and Main Roads (TMR), were recipients of a DAWE National Traceability Grant. The project team has developed a framework and traceability software platform currently being piloted within the Australian native seed industry. The framework and platform allow for all critical-tracking-events along the journey of a native seed batch to be easily captured utilising a smart phone application (APP) and the global standard for data capture. The platform provides a unique identification for each batch of seed and critical tracking event. The batch ID belongs to that batch and all supply chain stakeholders can contribute to batch traceability by providing more information/data to increase information integrity. This gives the end user, and other stakeholders, increased levels of trust in the product to support value, increase efficiency and reduce costs. For mining companies these efficiencies and cost reductions are in the form of information availability across site/company, potentially improved vegetation establishment, less rework and efficient monitoring. Ultimately this contributes to safe, stable and sustainable rehabilitation. By capturing data on harvest, logistics, storage (including temperature and humidity), aggregation/blending, treatment, application and ongoing management, the native seed industry and end utilisers of native seed have a greater level of product integrity, brand integrity and information integrity.

Aug 2, 2023

By J. W. Davis

In the last few years major industrial companies have begun to realize the importance of Reliability as an enterprise strategy that, properly implemented, will improve financial performance. Typical results of an effective Enterprise Reliability Strategy include a 20% -50% reduction in maintenance cost accompanied by a 5% - 10%increase in real production capacity, with no capital investment in production equipment. One factor fueling the race to acquire and implement enterprise reliability is the pressure for companies to be increasingly cost-effective and competitive in global markets. In a recent study, Asset Productivity: The Next Wave, the Boston Consulting Group (BCG)stated that, “In order to compete for funds, companies must offer investor returns that are competitive with other opportunities. Alternative investments such as dot-com and others with non-traditional business models have raised the bar.” (APDF version of the study can be downloaded at www.bcg.com). BCG views asset productivity as the most powerful mechanism for increasing shareholder return. The author believes that the most effective way to increase Fixed Asset Productivity is to maximize asset utilization by increasing the Reliability of the Assets and the associated processes. Developing and implementing an ERS requires significant effort and knowledge. Most companies have difficulty finding a sufficient supply of these valuable commodities to implement an ERS Program internally. Many companies also struggle with figuring out how to get started and what direction to proceed.

Jan 1, 2003

By F. Fraas, J. E. Conley

"The problem of recovering potash from the mineral polyhalite (K2SO4.MgSO4.2CaSO4.2H2O), occurring in large quantities in the salt beds of Texas and New Mexico, has been under investigation at the Nonmetallic Minerals Experiment Station of the U. S. Bureau of Mines continuously since 1928. Most of the results previously obtained have been published in technical journals and in a series of Bureau of Mines Reports of Investigations.The experiments described in the present report were performed to ascertain whether a continuous countercurrent extraction of calcined polyhalite by hot water would yield satisfactory recoveries and concentrations of sium sulphate in the top liquor. Previous investigation by Storch 4 had shown that the rate of solution of uncalcined polyhalite was too slow to be of value in an industrial process, and Storch and Clarke 5 had demonstrated that calcination of the polyhalite greatly, accelerated the rate of solution in hot water, allowing most of the potassium sulphate to be readily extracted."

Sep 1, 1933

By A. D. Marriott, J. V. N. Dorr

This paper reviews recent developments in the application of classification practice to the origination of fine-grinding flow sheets and traces the history of the mechanical classifier from its initial application for separating cyanide process sands and slimes down to its present six or more distinctly different applications at copper concentrators; it undertakes to show also, by reference to diagrammatic fine-grinding flow sheets and accompanying operating data from nine copper concentrators in western North America, the advantages gained from improved classi-ficiation flow sheets at these properties in terms of reduced grinding costs, improved flexibility of operation or increased recovery. Comparison is only made between different fine-grinding flow sheets at a given plant and no attempt is made to compare different concentrators, on account of ore variations and differences in metallurgical objectives sought,. The adoption of the flotation process in recent years, and especially the development of selective flotation, has brought a demand for much finer grinding than formerly. This has caused much thought to be given to grinding efficiency, and today there is hardly a mill where the grinding flow sheet is not under close study and subject to frequent changes. When closed-circuit grinding was introduced into metallurgy some years ago, its value was recognized at once, and since then the combination of mills and classifiers has been regarded and operated as a grinding unit. Apart from variations in both the grinding and classifying elements of this unit, there have been many variations in grouping tried by different mills to suit varying conditions of ore and plant limitations. Although operators feel that in most cases their present flow sheets are on trial, and the data on present work are often incomplete, we have felt that a discussion of the progress that has been made and an endeavor to show present trends and their results should be of use to the profession. We have therefore prepared flow sheets of some of the larger mills with which we have been in contact and present them with available data as to their results, in the hope that they may be of service now rather than later when practice may have become more standardized and more complete records and analyses have been made. We believe that the data given,

Jan 1, 1930

By Jean Viana Bahia, Antônio Adel dos Santos, Vicente Tadeu Lopes Buono

During cold rolling of Cr-Mo alloyed DP steel, considerable oscillation of thickness may occur. The literature points out that such occurrence is due to non-uniform cooling of the coil after the hot rolling process. Since the austenite transformation in this steel continues after coiling, the microstructure and, consequently, mechanical properties are very susceptible to natural variations in cooling rates associated with distinct positions of the coil. The influence of coil cooling conditions on thickness oscillation during cold rolling was evaluated in this work by using both industrial experiments and dilatometer tests. It was verified that an industrial coil presented large variation of mechanical properties associated with its heterogeneous microstructure. Consequently, thickness oscillation occurred during cold rolling. Dilatometer tests simulating hot run-out table and coil cooling showed that the austenite transformation is very slow under small cooling rates that occur after coiling. Thus, the slow transformation rate makes the coil very susceptible to environmental conditions around it during its natural cooling and is responsible for variation in mechanical properties of the coil. To ensure the formation of a more homogeneous microstructure in the whole coil, it is necessary either to make use of technologies that improves the cooling uniformity or to adjust the steel alloy design. The latter alternative has been done with relative success by using conceptions with lower amounts of Cr and Mo.

Oct 1, 2019

Solvent extraction has recently been introduced into Australian hydrometallurgical practice for the production of a high grade uranium concentrate from El Sherana ore by a sulphuric acid leach and solvent extraction process. The solvent is a 5 per cent solution of tri(iso-octyl)amine in kerosene modified with 4 per cent of a long chain alcohol. The stripping reagent is a molar solution of sodium chloride.Preliminary testing for the development of the process showed that the leach liquor was quite amenable to the solvent extraction process and that the equilibrium and rate considerations of both the extraction and stripping steps were very favourable.The industrial plant contains four stages of extraction, three stages of chloride stripping and one stage of secondary carbonate stripping. An internal type of mixer-settler is used for the stagewise contact, the design being based on tests with model equipment.The performance and control of the industrial plant is satisfactory; 99·7 per cent of the uranium is recovered for a loss of 0·3 gallons of kerosene and 0· 4 pounds of amine per 1,000 gallons of liquor treated.INTRODUCTIONThe processing of El Sherana uranium ore from the South Alligator River valley commenced in April, 1959, and thereby introduced into Australian hydrometallurgical practice the unit operation of solvent extraction on an industrial scale. Although there are now some twelve mineral processing plants in the United States and Canada using solvent extraction, its application to the field of primary hydrometallurgy is quite new. Prior to 1956 none of these twelve plants was operating and hydrometallurgical application waslimited to the refining of comparatively high grade uranium compounds and fission products from nitrate and nitric acid solutions.

Jan 1, 1961

By G. I. McPhail

The authors have conducted several investigations into the prediction of the beach profile of high-density tailings and have found that there are a number of important considerations that need to be taken into account over and above the reliability of the beach profile prediction methodology. These considerations relate to the chemistry of the slurry and specifically the influence of pH and flocculation, both of which have a significant influence on the rheology of the slurry at the discharge point. A number of examples are discussed and a potential testing protocol that will assist in assessing the influence of chemistry ahead of the beach profile predictions is presented. A methodology for assimilating the results of the testing into the likely field situation is discussed, and suggestions are made on application of the results in beach profile prediction. The suspected influence of residual flocculation on the stratification

Jan 1, 2012

By Karin Bäppler

A new polyhalite fertilizer mine is currently being developed in the UK by Anglo American Crop Nutrients. The project includes the construction of a Mineral Transport Tunnel almost 37 kms long to house a conveyor belt that will move polyhalite from the production shaft at the mine to a materials handling facility at the port. The project sets a new standard in terms of an ultra-long tunnel drive and sustainable, environmentally friendly and efcient material transport. The paper highlights in particular the . m diameter TBM in use for the construction of the ultra-long tunnelling section.

Jun 23, 2024

"This study examines the problems faced by open pit mine superintendents who make choices about how to direct their materials, either to the waste dump or to the mill. The paper explores the effects of introducing a 10% sampling error and a 0.9-times to 1.1-times sampling bias on positively skewed distributions for precious and base metals, negatively skewed distributions in the case of bulk commodities, and normal distributions as is the case for coal deposits. Parent distributions for each commodity were created on a 25 x 25 m grid using transformations of gold, iron ore, and coal data-sets, spatially based on a nonconditional Gaussian simulation. Ordinary kriging of grades for the three commodities into a 10 x 10 m grid provided the reference case against which the distributions with the sampling error and sampling bias for the commodities were compared. Imposing cut-off grades on the actual-versus-estimated scatterplots of the three commodities allowed the distributions to be classified into components of waste, dilution, ore, and lost ore. Ordinary kriging of values for each deposit type acted as the reference data-set against which the effects and influence of 10% sampling error and 0.9-times to 1.1-times sampling bias are measured in each deposit type. Indications are that the influence of error and bias is not as significant in gold deposits as it is in iron ore and coal deposits, where the introduction of small amounts of error and bias can severely affect the deposit value.IntroductionThe effects of poor sampling and the financial implications for mining companies, traders in mineral assets, and sellers of metal as dore or commodities is documented in a number of studies, the most notable of which is that by Carasco (2004). He examined the financial impact of poor sampling practices in the Chilean copper industry and found that finacial losses due to poor sampling amounted to hundreds of millions of dollars over the life of a mining operation. Holmes (2004) examined the effects of correct sampling and measurement as the foundations of metallurgical balances, and found that revenues from the sales of large iron ore shipments may be profoundly affected by poor sampling practices. In South Africa the way in which sampling of in situ gold-bearing reefs affects the mine call factor has been an ongoing study since the disparity between the estimation of gold in the reef and the actual gold bullion produced was noted by early investigators such as Beringer (1938), Jackson (1946), Sichel (1947), Harrison (1952), and a number of others."

Jan 1, 2017

By J. A. Eisele

The Federal Bureau of Mines is engaged in a continuing program on the recovery of alumina from domestic source materials. Of the six processes being studied, current efforts focus on HCl leach of clays. A key step in the HCI process is the removal of iron from the aluminum chloride leach liquor. This was accomplished .by solvent extracting the iron with a tertiary amine in kerosine to which decanol was added as a phase modifier. In a mixer-settler operation, iron in the raffinate was reduced to <10 ppm in two extraction stages from a feed containing 1.4 gil Fe. Iron was stripped from the organic phase in three stages with dilute HCl.

Jan 1, 1976

By Jürgen Kretschmann

Principally, mining natural resources is a finite business that reaches its limits once the deposits mined are depleted, the resources can no longer be mined in an economically profitable way or substitutes are pushing the mined products out of the market. An example of the latter is the increasing replacement of coal with natural gas and renewables in power generation in the United States [1]. According to the model of the product lifecycle, the global hard-coal mining industry has reached a stagnation phase [2]. The trend is obvious. Coal use peaked in 2013 [3], and the coal demand of China has been slowly decreasing since then [4]. Coal consumption in the United States saw a 16 percent decline from 726 Mt (800 million st) to 608 Mt (670 million st) between 2015 and 2019. In addition, according to the U.S. Energy Information Administration, it will not rise again [5]. The decline is attributed to complex market dynamics, from low gas prices because of the “shale gas revolution” [6] to federal environmental regulations like the Clean Power Plan. Moreover, important players like the United Nations and the European Union have already begun to describe pathways toward decarbonization. Increasing competition between coal-mining companies and the mining regions can be expected worldwide if companies want to keep their positions on the global and national coal markets. Companies will focus on the best deposits. European countries, like France, Spain or Germany, are only forerunners of this development — their centuries of coal production have passed. The concept of sustainable development (SD) is fundamentally based on a model of progress in which ecological, economic and social dimensions should be developed equally and positively. Questions arise, such as: How can SD be a corporate goal in a phase of decline? How can former mining regions sustainably progress to a better future? The steps Germany has taken to handle the coal decline in a sustainable way and the lessons learned from this process are described in this paper. 

By Santiago Gómez, Pablo Segarra, José A. Sanchidrián

In this paper, differences between the industry-standard Holmberg-Persson (H-P) approach and a semi-analytical vibration prediction model called full-field solution (FFS) are analized. The analysis is conducted at two levels: vibrations and rock damage.

Feb 1, 2020

By W. G. Davenport

Chapters 19 and 20 examine direcHo-copper flash smelting and flash converting. This chapter compares the two processes and suggests which is likely to be &apos;the more economic for a given concentrate. It: (a) uses Chapter 19&apos;s direct-to-copper industrial oxygen and oil requirements (b) adds the energy required for electric furnace recovery of Cu from direct-to-copper slag (Czemecki et al 1999) (c) combines Chapter 20&apos;s, flash converting calculations with Chapter 18&apos;s flash smelting calculations to determine their combined industrial oxygen and hydrocarbon fuel requirements (d) adds the energy required to granulate, crush and dry flash smelting matte for the flash converter (e) adds the energy required to granulate and dry flash converter slag for recycle to flash smelting (f) compares direct-to-copper and flash smelting/flash converting in terms of their total equivalent hydrocarbon ener.gy requirements.

Jan 1, 2001

By E. M. Porbansky

DURING the investigation of the electrical transport properties of copper, it became necessary to prepare large single crystals of the highest obtainable purity. In an effort to meet these demands, single crystals of copper have been grown by the conventional pulling technique—as has been used for the growth of germanium and silicon crystals.&apos; Low-temperature resistance measurements made on these crystals show that, as far as their electrical properties are concerned, they are generally of significantly higher purity than the original high-purity material. The use of these pure single crystals with very high resistance ratios has made possible the acquisition of detailed information regarding the electron energy band structure of copper2-&apos; and has stimulated widespread effort on Fermi surface studies of a number of other pure metals. It is the purpose of this note to describe our method of preparing very pure copper crystals by the Czochralski technique. Precautions were taken to prevent contamination of the melt from the crystal growing apparatus. A new fused silica growing chamber was used to prevent possible contamination from previous groqths of other materials such as germanium, silicon, and so forth. A new high-purity graphite crucible was used to contain the melt. This crucible was baked out in a hydrogen atmosphere at -1200°C for an hour, prior to its use in crystal growth. Commercial tank helium, containing uncontrolled traces of oxygen, was used as the protective atmosphere. A trace of oxygen in the atmosphere appears to be necessary for obtaining high-purity copper single crystals. A 3/8-in-diam polycrystalline copper rod of the same purity as the melt was used as a seed. The copper rod was allowed to come in contact with the melt while rotating at 57 rpm. When an equilibrium was observed between the melt and the seed (that is, the seed neither grew nor melted), the seed was pulled away from the melt at a rate of 0.5 mils per sec. As the seed was raised, the melt temperature was slowly increased, so that the grown material diminished in diameter with increasing length. When this portion of the grown crystal was -1 in. long and the diameter reduced to less than 1/8 in., the melt was slowly cooled and the crystal was allowed to increase to - 1-1/4 in. diam as it was grown. By reducing the diameter of the crystal in this manner, the number of crystals at the liquid-solid interface was decreased until only one crystal remained. Fig. 1 shows a typical pulled copper single crystal. The purity of the starting material and the crystals was determined by the resistance ratio method: where the ratio is taken as R273ok/R4.2ok. The starting material, obtained from American Smelting and Refining Co., was the purest copper available. Most of the pulled copper crystals had much higher resistance ratios than the starting material. The highest ratio obtained to data is 8000. Table I is an example of the data obtained from some of the copper crystals. Note that Crystal No. 126 had a lower resistance ratio than its starting material and this might be due to carbon in the melt. The melt of this crystal was heated 250" to 300°C above the melting point of copper. At this temperature it was observed that copper dissolved appreciable amounts of carbon. The possible presence of carbon at the interface between the liquid and the crystal will result in reducing conditions and negate the slight oxidizing condition required for high purity as discussed below. The possible explanations of the improvement in the copper purity compared to the starting material are: improvement in crystal perfection, segregation, and oxidation of impurities. Of these, the latter seems to be most probable. A study of the etch pits in the pulled crystals showed them to have between 107 and 108 pits per sq cm. The etch procedure used was developed by Love11 and Wernick.10 The resistivity of the purest copper crystal grown was 2 x 10-10 ohm-cm at 4.2oK; from the work of H. G. vanBuren,11 the resistivity due to the dislocations would be approximately 10-l3 ohm-cm, which indicates that. the dislocations in the copper crystals would contribute relatively little to the resistivity of the crystals at this purity level. Segregation does not seem likely as the reason for purification of the material, since the resistivity of the first-to-freeze and the last-to-freeze portions are approximately the same, as was observed on Crystal No. 124. On most of the crystals that were examined, the entire melt was grown into a single crystal. If the

Jan 1, 1964