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Coupled Reduction with Platinum Group Metals

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Coupled Reduction with Platinum Group Metals Coupled Reduction with Platinum Group Metals THE PREPARATION OF HIGH PURITY RARE METALS By U. Berndt, B. Erdriianii and C. Keller Institute for Radiochemistry, Karlsruhe Nuclear Research Centre presence of noble metals (platinum, palladium, Very pure metals of the actinide, rhodium, iridium) can be applied to prepare lanthanide and alkaline earth series can very pure noble metal alloys with actinide, be prepared from their oxides by lanthanide and alkaline earth elements, coupled reduction by hydrogen in the titanium, zirconium, hafnium, vanadium, presence of platinum group metals. niobium, tantalum, and even with lithium During the process the platinum group (2-6). metals form intermetallic phases with The direct synthesis of alloy phases of the metals from the oxides. These noble metals with base metals involves many phases are decomposed to yield the pure serious problems caused by the relatively metals in gaseous form and the platinum high vapour pressure of the base metals. In group metals in solid form. The pure addition, the choice of the crucible material gaseous metals condense to produce and of the gas atmosphere affects the results. pure solid specimens. Furthermore, ordered phases are obtained only by repeated homogenising and by pro- longed and careful annealing. Also the usual In the course of our investigations dealing methods of preparation of highly radioactive with phase equilibria in uranium oxide-rare metals are somewhat difficult, and in some earth oxide systems, we made the following cases the elements, such as protoactinium unexpected observations (I) : (islPa) and curium (244Cm),are only prepared (I) In fluorite phases with a high content of in milligram quantities and have not yet been rare earth oxides it is not possible to investigated sufficiently. Further methods for reduce higher valency states of uranium the preparation of intermetallic phases are to tetravalent uranium, at least when the reactions of platinum metals with using hydrogen and at temperatures nitrides (7,8), sulphides (9), borides (IO), below IOOC-IIOO~C. or carbides (II,IZ) of the base metals; the (2) At higher temperatures and when reactions of the carbides with platinum using noble-metal crucibles, we ob- metals have been investigated more served weight changes which indicated thoroughly. However, the results of the a reduction of the uranium to valencies reactions of base metal carbides with platinum below four. The metallic appearance metals do not give single-phase products of the reaction product made a chemical but mixtures, e.g. UMe, and U,MeC, reaction between the substance and the (Me=Ru, Os, Rh, Ir, Pt), or UMe, and crucible very possible. carbon corresponding to the initial metal Detailed studies proved this assumption concentration. The application of these and we were able to demonstrate that the methods to the preparation of intermetallic hydrogen reduction of metal oxides in the phases is further hindered, as the stoichio- Platinum Metals Rev., 1974, 18, (l), 29-34 29 metric constitution of the carbides or nitrides of hydrogen or ammonia. Reaction mech- must be examined by analyses before starting anisms of coupled reactions in the case of the the reaction. The preparation of the pure refractory oxides with practical reference to oxygen-free carbides and nitrides of the platinum thermocouples have been studied by transuranium elements is also complicated by Darling and his colleagues (15-19). practical problems. In the cases of curium Details of this method of obtaining the very and protoactinium no carbides and nitrides pure noble metal alloy-phases are as follows. have yet been prepared. When heating the oxides with finely powdered From metallurgical practice it is known noble metals in an extremely pure stream that oxides difficult to reduce are more easily of hydrogen, a reaction takes place which we reduced in the presence of nobler metals. have called “coupled reduction”, i.e. the re- This is the case for the preparation of ferrous duction of a metal oxide (carbonate)/fluoride alloys and results from the fact that with in the presence of a noble metal, leading to higher temperatures the oxygen partial the formation of a base metal-noble metal pressure of the oxide is raised by the presence alloy. of the more noble metal. Reduction is then The formula is general for the method used possible if both metals form mixed crystals (in the case of an oxide): and this is explained by the affinity forces xPt -1- Me,O + Hz S PtxMe,+HzO occurring during the formation of the mixed crystals (13). Up to the present time we have been able On this basis it was possible for Klemm to show that coupled reduction is possible and Bronger (14) to prepare some noble when using platinum, palladium, iridium and metal alloy phases by reduction of base metal rhodium as the noble metals. Attempts to oxides with platinum metals in the presence prepare alloy phases with ruthenium, osmium, Platinum Group Metal-Actinide Alloy Phases Prepared by Coupled Platinum Group Metal-Actinide Alloy Phases Prepared by Coupled Reduction during This Work I Reduction during This Work - Pu Am 3 U NP I n - ~_-Th Pa U - NP __ Pu %.Am - Cf - __ - Rh Rh,Pu Rh,Am Rh Rh,Pu Rh,Am "n Rh,Am 33 Rh,U Rh,Np Rh,Pu wa == Rh,Th Rh,Pa Rh,U Rh,Np Rh,Pu Rh,Am 'in Ir Ir,Npa Ir,Pua Ir2Arna Ir Ir,Npa Ir,Pua Ir,Cma Ir,U ... Ir,Pa Ir,U. .- - - - Pd Pd,Np Pd,Pu Pd,Am Pd Pd3NP Pd,Pu Pd,Am Pd,Cm Pd,Th Pd,U Pd,Th I Pd,U Pd,U Pd,U Pt Pt,Pu Pt,Arn Pt Pt,Pu Pt,Am Pt,Cm Pt,Thb Pt,Pa Pt,U Pt,Np Pt,Pu Pt,Thb Pt,Pa Pt,U Pt,Np Pt,Pu Pt,Th Pt,Pa Pt,U Pt,Np Pt,Pu Pt,Arn Pt,Th Pt,Pa Pt,U Pt,Np Pt,Pu Pt,Arn Pt,Cm (Pt,Cf)c a No Ir,A tcompounds exist a No Ir,A compounds exist b Not obtained in pure form b Not obtained in pure form c Only indirect proof c Only indirect proof Compounds in bold type were prepared for the first time Compounds in bold type were prepared for the first time Platinum Metals Rev., 1974, 18, (1) 30 nickel, or cobalt by means of coupled re- duction have been started. The temperature needed to achieve complete reduction in- creases when going from platinum to iridium and decreases with increasing atomic number of the actinide element. Furthermore, alloys with a high noble metal : actinide ratio are more easily prepared than compounds having a lower ratio. This means, for example, that Pt,Cm may be prepared at about 12oooC, whereas the preparation of the iridium compound requires temperatures of 1550°C. The table shows the platinum-, palladium-, iridium-, and Rh-actinide intermetallic phases prepared by coupled reductions, among them the twenty com- pounds prepared for the first time. Intermetallic Phase Structure The structure of PtjA phases (A=Th, Np-Cm) was elucidated by comparison with compounds of the Pt,RE type which were prepared by coupled reduction and were investigated by Bronger (20). The hitherto unknown structure of Pt,Th and Pt,Pu proved to be isostructural with Pt,Sm; Pt,Pa and PtjU crystallise in the cubic Ni,U-structure type. The structure of the other new alloy phases could be established by comparison with known types of structures. The 2:1 compounds crystallise in the cubic Laves- phase type, whilst most 3:r phases have the ordered Cu,Au-structure type. Deviation from this structure type could be observed only for the platinum alloy phases of the light actinide elements. Four different types of structures were found for the 3:r com- thanide or the actinide series has the same pounds of the platinum system. Pt,Th is the stoichiometric formula but different lattice only compound whose type of structure is structures. The structures of these different unknown. The Pt,Pa and Pt,U alloy phases lattice types, however, are very similar, only crystallise in the hexagonal Cd,Mg-structure the stacking order being different. The type, Pt,Np has the hexagonal Ni,Ti- lattice constants of the isostructural series lattice, while the Pt3Pu phase has the ex- follow a trend which is generally known pected Cu,Au-structure type. This fact is when comparing the radii of the actinide remarkable because no case has been reported elements. In the case of the Ir,A (A=Th, as yet in which a simple compound of three U-Cm) and Rh3A (A=Th-Cm) com- neighbouring elements in either the lan- pounds this may be seen in Fig. I. A mini- Platinum Metals Rev., 1974, 18, (1) 31 mum in the lattice constants is to be Seen measured with an “Hygrometer PA 1000’’ between uranium and neptunium, both made by Panametrics, Waltham, U.S.A. of which metals have been shown to possess The same method was also used to purify the highest valency in their metallic state. helium and argon, which sometimes were used Such a dependence of molar volume with as inert gas when cooling reaction products, the atomic number could not be observed in Coupled reductions for the preparation of the series of platinum compounds because most of the platinum alloy phases and all of of the different types of structures, having the palladium, iridium and rhodium alloy more or less dense packing of the atoms. phases were unsuccessful when performed The preparation of the Pt,RE phases with two commercial hydrogen diffusion (RE =La-Tm, Y) by coupled reduction was apparatuses (3).
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