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The Properties of Zirconium and Its Possiblilities for Thermal Reactors

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The Properties of Zirconium and Its Possiblilities for Thermal Reactors -ASSI F' .... f""\ ~TRAL RESEARCH LIBRAB' Eel- . ;ik-:,3 ,~CUMENT COr.LECTION ORNL 228 IUACTORS ~lili~il~l~i~lj~illiii~rlllflrllf~r ~)~i~i 'llrll 3 4456 0360370 4 .\!J ORNL'!'>2~6 Reuctor~ '" \ , This dOGument consists~ .tl pages~ '. • .... CO?Y 5 arl05 Seri~s A• Issued I ~ - !fcJt;~ C'ontrnct No., \\""1"7405. eng 26 _.__ ,__ ~~ ____ TIlE lJROPERTIES OF ZIRCONIU'..K "!' ~AND ITS _,POSSIBILITIES FOR THERMAL R;EACTORS By Harold B, Fairchild of the Power ~ile Division \~ ~ DATE ISSUED JAN 7 194,9 OAK RIDGE NATION1~ LABORAT0RY OPER1~TED DY Carbide & Curbon Cheniculs Corporation for the Atomic Energy Cormnission lllrm~li~~lll~rltl .t?ust Office Box }:l Oak Ridge, Tennessee 3 4456 0360370 • .".. __ r~"" .-~. ~ • " p. !~ I ...., l~~ '-'I'" .. '" OJ (.. • \...;:~ I!::::; ~ :., = -----...- - ,. ~ ORl'lL~226 Reactors DISTRIBUTION ~ 1. 2 ... 4. .... 6 • 6. 1. 8~' 9""i'12. 13. H. 15~ ~6. 17. 18 111 19. 20. 21 tt 22. A. 23. S. 24. 25. 26. 27. 28. 29. 30.. 31. 32. 33. 34. 35-36. 37. 38. 39-56. Laboratory 57-58. ommissivn. ~ashington . '59~ a1 Institute 60 ..65~ onal Laboratory 66. 67. s 0ffice 68-71. Company, Riohland '72. s affi~e 73 74-7 Laboratory 78 l'v'ilssaohusetts lnt\:itute of Technology (Kaufmann) NEPIi. i'roject New York Opera North .hmeriCanAvi~· on, J,no • .t?atent Branch, Vias ,gtc:m Technical lnforIT'''; tl Division ORaO =w.:"'.I.l>-lof Qulif(jrn~a R~~diati0n Laboratory the 3 ~ Q! ..-;,.CQ;;;.;;;NT=m'I;;.,;:T;.;;..S Page No ... Introduction 5 I. The History of Zirconium. 6 II. ,The Abundance of Zirconium. 7 III~ The Physical and Atomic Constants of Zirconium 8 Including Properties Other Than Mechapicnl. IV. The Mechanical Properties of Ziroonium. 15 V. The Nuclear Physics Properties and the Effect of 25 Hafnium in Zirconium. VI.·The Production of the Ductile Zirconium Metal. 30 VII. The Production of -ZirconiUm Powder. 38 VIII.· The Fabrication of Zirconium. 39 IX. The Chemical Beactivity of ZirconiUn. 42 X. The Corrosion Besistonce of Zirconium. 55 . XI. The Separation of Hafnium f'romZirconium. 64 XII.' The Methods of Analysis for Dete:rmlng Hafnium in Zirconium. 73 XIII.' The Effects on Various Froperties of Zirconium by a Few Miscellaneous Impurities. 81 XIV. The Suitability of,Zirconium for Thermal Reactors 82 XV. The Plating of Ziroonium on Other Materials. 88 Bibliography 91 Appendix 99 , -~ ----~- 4 .: ' ..... ~ LIST OF ILLUSTRATIONS " Figure No. Page No. ... 1. Paramagneti,c Suaceptibility of Zirconium as a . Function of Temperature. 14 2. Graph by L. J. Rainwater and 'iN. Vi. Havens I Jr. Showi~ Slow Ne~tron Transmission of 0.16 gm/cm2 of Hafnium. 28 3· Graph by L. J. Rainwo.ter and 'iN. Vi. Havens, Jr. Showi'!tS Slow Neut:ron Transmission of 6.45 2 2 gm/cm of zr02 and 0.16 gm/cm of Ha:fnium. 29 4. Pyrex Glaes Apparatus for the Preparation of , Iodide Deposited Zirconium. 32 5~ Arc Furnace for the Production of Zirconium 'Carbide. 33 '6 •. Apparatus for Producing Dense Zirconium Chloride. , 34 7. FloW' $heet of Process for Preparing Pure Zirconium • in Bureau of Mines • 35 8. Apparatus Used by Lilliendahl and aentschler to 'Produce Pure Zirconiun. 36 9. Vacu'¥I1 ~intering Furnace for Zirconium. 37 10. Absorption of Oxygen by Zi:rconium. 50 11. Gain in. Weight of Zirconium on Heating in Air (Foote Crystal Bnr) ~l 12. Absorption of Nitrogen by Zirconium. 52 13. Absorption of Hydrogen by Zircon!um (J. D. Fast). 53 14. Absorption of Hydrogen by Zirconium (Bukagawo. and Nambo) 54 15 . Detroit Edison Test Speoimens 61 16. A Comparison of the Corrosion and Corrosion Rates for Two Kinds of Zirconium in Demineralized (nndProbably Air Saturated) Water at 3150 C. 62 17. Graph Showing Corrosion of Three Spec~mens of Foote Mineral (Iodide Depoei ted) Zirconiun p.t 0 C , 315 ~ in Air Saturated Demineralized Water. 63 18. Apparatus for the Determination of Oxygen ~nZr. 102 5 INTRODUCTION ... Up ~ntil about a year ago, zirl;::ori'ium had not been serioUsly considered for reactor uses because of an apparently 'high absorption cross section to thermal neutrons. New oross section measUrements Qn pure zirconium made , during the vintel;" of 1947-48, howevf,l,r" showed that :the apparently high croas seotion of zirconium was not due :to zirconium, but to the element hafnium, which co-exists with zirconium an~ is so similar to, zirconium in chemical properties that it cannot be separated by ordinary chemical methods. Since this discovery, great interest has been taken by various laborator~e8 opera1?ed for 'the Atomic Energy Commit;lsion throughout the country in the devel(i>':" ment of the metallurgy of a ,ductile zirconium and in the development of processes for the separation of 'the undesirable element, 'hafnium. The Power pile Division of th~Oak Ridge National Laboratory has completed a study of the water·cooled and water-moderated power reactor for the propulsion of naval craft, viz. submarines (see ORNL-133). As was anticipated, many problems in the deaign of a water-coo~ed reactor became apparent, among which one of the greates~ of these was the choice of a structural material which .woul4, resist, the corrosive effect of high temperatuve, high pressure water containing dissolved oXygen, hydrogen, and perhaps hydrogen peroxide, . Therefore, since zirconium was known to have good corrosion resistance to . aque,ous solutiona and had just been discovered to be desirable from a nuclear v~ewpoint, a' stu4.y of the possibilities of this metal as a structural material for a water-cooled reactor was undertaken. This investigation included l} the collecting of many facts concerning zirconium beginning with the history of the metal, 2) the compiling of information relative to its properties, its production} anQ,. its fabrications, hafnium separation processes, and co;rros:i,on studies. This ,report was prepared as a convenient reference f?r those who may be interested in any or all of these branches of !nvestigationee~cerning zirconium, 6 CHAPTER I THE HISTORY OF ZIRCONIUM 1 .. The recorded disco~ery of zirconium dates back to 1789 when Klaproth, in analyzing a precious stone known as Jargon from Ceylon discovered what he thought to be a. new earth and called trZirconerde". Other investiga.tors confirmed this. discovery in the minerals now known as zirconium ores. How­ ever, it was not until 1824 that anyone was able to reduce the metal from the oxide. 'Berzelius accomplished this,. producing the first known zir90ni­ tum· metal, though quite impure. Other Uelements" such as sonorium,. JargoniUJn, nigrium, euxeniu.in were reported to exist in zirconium oxide but only the element hafnium really proved to exist. Bohr predicted in 1922 in conclusion from his theory of atomic structure that zirconium was not an earth as Klaproth had thought ahd did not belong to the rare earth group but that it was quadrivalent and theref~re the direct homologue of zirconium. Since the X-ray spectrum of zirconium could be predicted, Coster and van Hevesy investigated various zirconium ores by X-r~y spectroscopy and substantiated Bohr's conclusion. Coster and van Hevesy also discovered the presence in the zirconium ores of the new element hafnium suggested by the Latin name Hafnia, for Copenhagen, where the discovery of the element was made following its earlier pIQduction there. f 7 Chapter II THE ABUNDANCE OF ZIRCONIUM1,2,3 The aarth,'g crust has been estimated to oontain 0.028 per cent zirconium, a figure which 'indicates that ziroonium is more abundant than the oommon metals nickel (.020 per.cent), oopper (.010 per oent), zinc (.004 per cent) and lead (.002 per cent). Ziroonium hae been known as a rare metal because of the difficulty of extracting the pure metal from the ores just as aluminum was conside~ed rare before the days of the development of the electrolytic method 'now used in its production. ,The most abundant zirconium bearing mineral is the are "zirc911t!, ZrSiO , which crystallizes in the tetragonal system and is isomorphous with rqtile,4 'Ti02 , The transparent yellowish or reddish varieties of the silicate are known as the precious stone hyacinth, and the colorless silicate as jargon. Other zirconium eilicate'bearing ores are alvite, malacone and cyrtol1te. Zirconium is not only found as the silicate but as the oxide. The , Brazilian: mineral, baddeleyite, is a fairly pure oxide, Some silicate is often faund with the oxide. Commercially the BraZilian mineral is called , "zirkite". ' ZirconiUm. ores contain varying amounts of hafnium, an element which is almost identical to Zirconium in all its chemical properties but differs in its nuclear properties in that it has a very high cross section to thermal neutrons, a high atomic weight and higll density. The hafnium/zirconium ratiQ by weight of the many' zirconium bearing ores range from'less than, 1 per cent in the BraZilian baddeleyite to 54 per cent in the cyrtol1te fo~d' in some' localities in the United States, probably t1+e feldspar mine in Bedford, N.Y., . and 54 per cent in the alvi'tfe minerals of Kraero. Three per cent 18 Ii more average figUre, however~ In the western hemisphere, the zircon sands of Florida cohtains about 3.3 per cent hafnium and 1;he zir~ite of B~az1l .about 0.7 per cent. 8 CHAPTER III THE PHYSICAL AND ATOMIC CONSTANTS OF ZIRCONIUM INCLUDING PROPERTIES OTIJEa THAN MECHANICAL* The element 'zirconium is the fortieth element' in the periodic table and has been assigned the atomic weisht of 91.22 by the International union of Chemists in 1935. It has a grain structure of hexagopal close-packed crystal below 865° c** in the a phase~ a body~centered cubic crystal 0 structure above 865 C in the ~ phase.
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