Cadmium, zinc and lead are constituent components of many semiconductor compounds. The obtained high purity distillates and ingots are large-size elements, which is not always convenient to use, and thus require additional grinding, which does not always allow maintaining the purity of the original materials. For the growth of semiconductor and scintillation single crystals it is advisable to use «friable» granular high-purity distillates, which can be processed without the risk of contamination. For example, the European low-background experiment LUCIFER required more than 20 kg of high-purity granulated zinc, which was agreed to be supplied by NSC KIPT. This task was then extended to cadmium and lead. Motivated by these tasks, the authors of this paper propose complex processes of deep refining of cadmium, zinc and lead by vacuum distillation. A device producing granules has been developed. The process of granulation of high-purity metals is explored. The purity of produced granules for cadmium and zinc is >99,9999, and >99,9995% for lead granules. To prevent oxidation of metal granules during exposition to air, chemical methods of surface passivation were used. Organic solvent based on dimethylformamide used as a coolant improves the resistance of granules to atmospheric corrosion during the granulation of high purity Cd, Zn and Pb.
The production of ultra-pure raw material is a crucial step to ensure the required background level in rare event searches. In this work, we establish an innovative technique developed to produce high-purity (99.999%) granular zinc. We demonstrate the effectiveness of the refining procedure by measuring the internal contaminations of the purified zinc with a high-purity germanium detector at the Laboratori Nazionali del Gran Sasso. The total activity of cosmogenic activated nuclides is measured at the level of a few mBq/kg, as well as limits on naturally occurring radionuclides are set to less than mBq/kg. The excellent radiopurity of the zinc sample allows us to search for electron capture with positron emission and neutrinoless double electron capture of $$^{64}$$ 64 Zn, setting the currently most stringent lower limits on their half-lives, $$T_{1/2}^{\varepsilon \beta ^+} > 2.7\times 10^{21}~\text {year}$$ T 1 / 2 ε β + > 2.7 × 10 21 year (90% CI), and $$T_{1/2}^{0\nu 2\varepsilon }> 2.6\times 10^{21}~\text {year}$$ T 1 / 2 0 ν 2 ε > 2.6 × 10 21 year (90% CI), respectively.
A process has been developed to produce high-purity granular zinc for growing Zn82Se scintillation crystals de-signed to study the neutrinoless double beta decay (0ν2β) of the selenium isotope 82Se in the CUPID-0 experiment. The chemical and isotopic compositions of high-purity zinc were studied and its radioactive purity was evaluated. At a level less than mBqkg-1 in the background spectrum of high-purity zinc, measured by a germanium detector, no peaks were observed for natural radionuclides 40K, 60Со, 137Cs and the uranium-thorium decay chain. An in-creased activity of such nuclides as 54Mn, 56Со, 57Со, 58Co, and 65Zn, formed mainly due to cosmogenous effects, was noted.
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