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Oxidation Studies of Some Refractory Metals James Henry Witte Iowa State University

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Oxidation Studies of Some Refractory Metals James Henry Witte Iowa State University View metadata, citation and similar papers at core.ac.uk brought to you by CORE provided by Digital Repository @ Iowa State University Ames Laboratory Technical Reports Ames Laboratory 2-1964 Oxidation studies of some refractory metals James Henry Witte Iowa State University Harley A. Wilhelm Iowa State University Follow this and additional works at: http://lib.dr.iastate.edu/ameslab_isreports Part of the Metallurgy Commons Recommended Citation Witte, James Henry and Wilhelm, Harley A., "Oxidation studies of some refractory metals" (1964). Ames Laboratory Technical Reports. 66. http://lib.dr.iastate.edu/ameslab_isreports/66 This Report is brought to you for free and open access by the Ames Laboratory at Iowa State University Digital Repository. It has been accepted for inclusion in Ames Laboratory Technical Reports by an authorized administrator of Iowa State University Digital Repository. For more information, please contact [email protected]. Oxidation studies of some refractory metals Abstract Samples of niobium, tantalum, molybdenum and tungsten metals have been given phosphided cases by heating in a phosphorous atmosphere. The as mples were subsequently exposed to air at an elevated temperature. In tests at 800°C, the phosphided samples resisted air oxidation markedly compared to the pure untreated samples. The hospp hided cases were only a few microns thick yet oxidation resistance of all these samples extended for several hours. Phosphided samples with 90° edges did not resist oxidation at the edges as well as rounded edge samples. Disciplines Metallurgy This report is available at Iowa State University Digital Repository: http://lib.dr.iastate.edu/ameslab_isreports/66 IS-854 IOWA STATE UNIVERSITY OXIDATION STUDIES OF SOME REFRACTORY METALS by James Henry Witte and Harley A. Wilhelm RESEARCH AND DEVELOPMENT REPORT U.S.A.E.C. ADl GROOM­ -t:tXSICAL SCIE ]CES RE . IS-854 Metals, Ceramics and Materials (UC -25) TID 4500 May 1, 1964 UNITED STATES ATOMIC ENERGY COMMISSION Research and Development Report OXIDATION STUDIES OF SOME REFRACTORY METALS by James Henry Witte and Harley A. Wilhelm February, 1964 Ames Laboratory at Iowa State University of Science and Technology F. H. Spedding, Director Contract W -7405 eng-82 2 IS-854 This report is distributed according to the category Metals, Ceramics and Materials (UC-25) as listed in TID-4500, May 1, 1964. r-------- LEGAL NOTICE----------, This report was prepared as an account of Government sponsored work. Neither the United States, nor the Commission, nor any person acting on behalf of the Commission: A. Makes any warranty or representation, expressed or implied, with respect to the accuracy, completeness, or usefulness of the information contained in this report, or that the use of any information, apparatus, method, or process disclosed in this report may not infringe privately owned rights; or B. Assumes any liabilities with respect to the use of, or for damages resulting from the use of any information, apparatus, method, or process disclosed in this report. As used in the above, "person acting on behalf of the Commission" includes any employee or contractor of the Commission, or employee of such contractor, to the extent that such employee or contractor of the Commission, or employee of such contractor prepares, disseminates, or provides access to, any information pursuant to his employment or contract with the Commission, or his employment with such contractor. I Printed in USA. Price $ 1. 00 Available from the Office of Technical Services U. S. Department of Commerce Washington 25, D. C. 3 IS-854 TABLE OF CONTENTS Page ABSTRACT . .............................-. 5 I. INTRODUCTION . 6 II. HISTORICAL AND LITERATURE SURVEY................ 6 III. MATERIALS. 9 IV. SPECIMEN PREPARATION............................. 12 A. Fabrication of the Refractory Metal.................. 12 B. Phosphide Case Preparation . • . • • . • . • . • 13 V. OXIDATION TESTS .•....•.••...· •..•...•..•..•••........ 17 VI. RESULTS . 21 VII. DISCUSSION. 36 VIII. LITERATURE CITED.. • . • . • . • . • . 37 4 IS-854 IS-854 5 -·- OXIDATION STUDIES OF SOME REFRACTORY METALS_,_ James Henry Witte and Harley A. Wilhelm ABSTRACT Samples of niobium, tantalum, molybdenum and tungsten metals have been given phosphided cases by heating in a phosphorous atmosphere. The samples were subsequently exposed to air at an elevated temperature. In tests at 800°C, the phosphided samples resisted air oxidation markedly compared to the pure untreated samples. The phosphided cases were only a few microns thick yet oxidation resistance of all these samples extended for several hours. Phosphided samples with 90° edges did not resist oxidation at the edges as well as rounded edge samples. * This report is based on an M.S. thesis submitted by James Henry Witte, February, 1964, to Iowa State University, Ames, Iowa. 6 I. INTRODUCTION There is an increasing need for high strength materials that will withstand oxidizing atmospheres at the higher temperatures required for the operation of power generators designed for increased thermal efficiencies desired in atomic, space and conventional engines. A great majority of the refractory metals (those having desirable high-temperature strength) will not withstand an oxidizing atmosphere for any appreciable length of time at temperatures as low as 1000°F. It is known that many alloys are less susceptible to oxidation than their basic components. There is the possibility then of treating a refractory metal to obtain an oxidation resistant composition on its surface. The present investigation is based on a study of the formation of case-phosphided metals and on a study of the oxidation resistance of such treated metals . Due to the breadth of these areas of study, the present investigation has been limited to the phosphiding of the refractory metals niobium, tantalum, molybdenum and tungsten and to the oxidation behavior of the treated and untreated metals. For the purpose of obtaining an indication of the effectiveness of the phosphiding treatment on these metals ·' oxidation tests were made in a stream of dry air at a temperature of 800°C (1470°F). II. HISTORICAL AND LITERATURE SURVEY In recent years work toward the development of high strength materials that will withstand an oxidizing atmosphere at elevated temperatures has been conducted in many laboratories. The oxidation behavior and other 7 characteristics of a number of metals have been extensively studied (1, 2, 3). Four refractory metals, niobium, tantalum, molybdenum and tungsten have been most prominent in such studies. However, very little information relative to the preparation and oxidation behavior of phosphided cases on these four metals could be found in the literature. Phosphide cases have been prepared on a number of metals by the direct reaction of elemental phosphorus vapor on the massive metal. Investigators at the Nuclear Corporation of America (4) have prepared phosphide cases on sheets of four refractory metals, yttrium, zirconium, hafnium and molybdenum by this means at temperatures ranging between 600° and 1000°C. Although the phosphiding treatment was for periods of up to 20 hours, no values of total phosphorus pick up or phosphide case thickness were reported. Powdered metal phosphides have been prepared by reaction of the powdered metal with phosphine (5). It appears then that phosphide cases could also be prepared by the use of phosphine on massive metal. The refractory metals with phosphide cases prepared by workers at the Nuclear Corporation of America were tested in an oxidizing atmosphere at 1000°C. It was found that phosphiding decreased the rate of oxidation for short periods of time at this temperature. For molybdenum the period of depressed oxidation was about 3 hours. In the case of yttrium and hafnium the decreased rate lasted about 8 hours and for zirconium about 16 hours (4). The oxidation behavior of the untreated refractory metals of interest here has been found to follow certain relationships that depend on the 8 temperature range of oxidation. The rate relationships used to describe most oxidation behaviors are of the general form (.6m/a)n=Kt (6) where .6m/a is weight gain or loss per unit area, in time t at temperature, and K is a constant that depends on the metal and its environment. The value of n may or may not be a constant for a metal over a range of tempera­ tures. No such mathematical relationship was proposed in the report of the Nuclear Corporation of America for expressing the oxidation behavior of phosphided metals. The data supplied in the report are inadequate for the period of depressed oxidation to uniquely define the behavior mathematically. It is possible that after the period of depressed oxidation, the behavior resembles that of the untreated metal. The form of the rate relationship is determined by the numerical value of n. In the case of a linear rate relationship the value of n is one, for parabolic and cubic the values of n are two and three respectively. When n varies between one and two over a temperature range the behavior is described as a combination of linear and parabolic (6). The relationship that best represents the oxidation behavior of niobium is parabolic at temperatures not above 300°C. The oxidation behavior transforms to a linear relationship at temperatures of 700°C and greater, a combination of the parabolic and linear applies in the 300° to 700° C (7). The oxidation behavior of tantalum transforms from parabolic at temperatures below 500°C to linear at temperatures of 7.00°C and above. Between 500° and 700°C the oxidation is a combination of parabolic and 9 linear relationships (8). When molybdenum oxidizes it forms a volatile oxide and loses weight with an increase in time. Thus, the value of 6.m/a for molybdenum is negative. However when the oxidation rate relationship is formulated only the absolute value of 6.m/a is employed. The oxidation of molybdenum follows a parabolic relationship at temperatures not above 275°C. From 27 5° to 700° a combination of parabolic and linear relationships 1s observed and above 700°C the oxidation follows linearity (9).
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