“Leading Scientific Research Institute of Chemical Technology” JSC, Moscow, Russia.

M. L. Kotsar, Head of Laboratory, phone: +7 (499) 324-63-75
S. A. Lavrikov, Leading Researcher
A. O. Lapidus, Leading Engineer

“Chepetsky Mechanical Plant” JSC, Glazov, Udmurtia, Russia.

E. V. Ilenko, Head of Central Scientific-Research Laboratory
A. V. Aleksandrov, Head of a Group of Central Scientific-Research Laboratory

This article considers the preparation of circulating raw materials to iodide refining of hafnium in multiple shell metallic apparatuses by the following methods:
— vacuum annealing (fused tablets, shavings);
— hydroflouric-nital etching (fused tablets, hafnium shavings, groats of hafnium-nickel ligature of the GFN-10 (ГФН-10) grade);
— ultrasonic machining with cleaning agent (shavings, fused hafnium tablets).
In sum, more than 50 kg of circulating raw materials was processed in laboratory conditions. The most complete removing of surface product layer takes place during the etching of circulating materials by acids mixture. At the same time, there takes place the significant transition of the basis into the etch solution, especially during the processing of shavings (to 37.5%) and ligature (to 11.4%). There is also required the extraction of hafnium from solutions in the form of fluoride compounds with its following return into the technology. Ultrasonic machining with powerful cleaning agent is the most modern and ecologically pure method of preparation of circulating raw materials. There was researched the process of compacting of circulating shavings of variable size hafnium. This process was carried out by the pressing of tablets with diameter of 1.4–2.0 mm in the pressure range of 290–955 MPa, and by agglomeration of these tablets in vacuum with the residual pressure of ~0.13 Pa and temperature of 1500 ^оC. There is substantiated, that density and durability of agglomerated tablets depend on the coarseness of shavings and compacting pressure. As a result of experiments, there were obtained the agglomerated hafnium tablets, which pressing density and durability are 74–79% (from theoretical), and 562–625 MPa. For the purpose of preparation of circulating hafnium shavings to iodide refining, the water washing, drying, heating and vacuum annealing are used in industrial conditions in the temperature range of 850–950 ^оC during 6 hours. There were carried out the experiments of circulating raw materials during the iodide refining of hafnium in metallic apparatus with deposition of metal on the hairpin-filament. There was researched the chemical composition of iodide hafnium bars from initial and circulating raw materials. In both cases, chemical composition of the bars is much the same.

1. Kotsar M. L., Morenko O. G., Shtutsa M. G., Akhtonov S. G., Aleksandrov A. V., Ziganshin A. G., Indyk S. I., Kucheryavenko E. N., Lazarenko V. V., Lapidus A. O., Pogadaev V. A., Popov A. M. Neorganicheskie materialy — Inorganic Materials. 2010. Vol. 46, No. 3. pp. 332–340.
2. Kotsar M. L., Lavrikov S. A., Nikonov V. I., Aleksandrov A. V., Akhtonov S. G., Aleksandrov A. V. Atomnaya energiya — Atomic Energy. 2011. Vol. 111, Iss. 2. pp. 72–77.
3. Moiseev V. G., Morenko O. G., Pogadaev V. A. et al. Apparat dlya iodidnogo rafinirovaniya tsirkoniya (Apparatus for iodide refining of zirconium). Patent RF, No. 2261287, MPK С 22 В 34/14, С 22 В 9/10. Applied : November 06, 2003. Published : September 27, 2005.
4. Aleksandrov A. V., Antipov V. V., Ziganshin A. G., Moiseev V. G., Morenko O. G., Pogadaev V. A., Shtutsa M. G., Kotsar M. L. Apparat dlya iodidnogo rafinirovaniya gafniya (Apparatus for iodide refining of hafnium). Patent RF, No. 2353687, MPK С 22 В 34/14, С 22 В 9/00. Applied : October 31, 2007. Published : April 27, 2009.
5. Shikov A. K., Bocharov O. V., Arzhakova V. M., Bezumov V. N., Perlovich Yu. A., Isaenkova M. G. Metallovedenie i termicheskaya obrabotka metallov – Metal Science and Heat Treatment. 2003. No. 8. pp. 20–23.
6. Evstyukhin A. I., Leontev G. A., Kotsar M. L., Bateev V. B., Zarembo Yu. I., Khvostova I. F. Ochistka ot primesey v protsesse iodidnogo rafinirovaniya gafniya i ego splavov s nikelem. Konstruktsionnye materialy v atomnoy tekhnike (Decontiminating during the process of iodide refining of hafnium and its alloys with nickel. Construction meterials in atomic engineering). Sbornik nauchnykh trudov “MIFI” (Collection of Scientific Proceedings of National Research Nuclear University “MEPhI”). Moscow : Energoatomizdat, 1987. pp. 15–24.
7. Bateev V. B., Evstyukhin A. I., Kotsar M. L., Leontev G. A., Ryabin E. V., Fedorov V. D. Sposob polucheniya tsirkoniya ili gafniya vysokoy chistoty (Method of obtaining of zirconium or high purity hafnium). Patent RF, No. 2048558, MPK С 22 В 34/14. Applied : April 12, 1993. Published : November 20, 1995.
8. Godneva M. M., Motov D. L. Khimiya ftoristykh soedineniy tsirkoniya i gafniya (Chemistry of zirconium and hafnium fluorides). Leningrad : Nauka, 1971. 115 p.
9. Gmurman V. E. Rukovodstvo k resheniyu zadach po teorii veroyatnostey i matematicheskoy statistike (Guidance to the solving of tasks of probability theory and mathematical statistics). Moscow : Visshaya shkola, 1970.
10. Baryshnikov N. V., Geger V. E., Denisova N. D., Kazayn A. A., Kozhemyakin V. A., Nekhamkin L. G., Rodyakin V. V., Tsylov Yu. A. Metallurgiya tsirkoniya i gafniya (Metallurgy of zirconium and hafnium). Moscow : Metallurgiya, 1979. pp. 172–181.