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Production of Germanium Stable Isotopes Single Crystals

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Production of Germanium Stable Isotopes Single Crystals Cryst. Res. Technol., 1700026 (2017) / DOI 10.1002/crat.201700026 Production of germanium stable isotopes single crystals Mihail Fedorovich Churbanov1, Vladimir A. Gavva1,∗, Andrey D. Bulanov1, Nikolay V. Abrosimov2, Eugeniy A. Kozyrev1, Ivan A. Andryushchenko1, Victor A. Lipskii1, Sergey A. Adamchik1, Oleg Yu. Troshin1, Artem Yu. Lashkov1, and Anatoly V. Gusev1 Original Paper Received 15 February 2017, revised 23 March 2017, accepted 23 March 2017 Published online 7 April 2017 for quantum calculations is actively investigated [6, 7]. It is reported on production of germanium stable isotopes It is also one of the purest elements produced in solid 72Ge, 73Ge,74Ge,76Ge single crystals with high isotopic and single crystalline state. Germanium tetrachloride is used chemical purity by hydride method. Separation of isotopes as the initial volatile compound in technology of produc- was carried out by centrifugal method using monoger- tion of semiconductor germanium. mane as the initial volatile substance. Samples of monoiso- Centrifugal method is an efficient method for sepa- ration of isotopes [8]. While using GeCl for centrifugal topic monogermanes 72GeH , 73GeH ,74GeH , 76GeH were 4 4 4 4 4 separation of germanium isotopes, the problems appear purified by the method of low-temperature rectification. connected with the so-called «isotopic overlapping» due Elementary polycrystalline germanium was extracted by py- to the fact that chlorine is of not monoisotopic nature rolysis from respective monogermane and purified from im- and comprises the mixture of two stable isotopes 35Cl purities by the method of zone melting. Single crystals of and 37Cl. It decreases the extraction coefficient of the tar- germanium isotopes were grown by Czochralski method. get product and limits its isotopic purity. That is why The content of the main isotope in the produced single crys- germanium tetrafluoride is used as the initial volatile tals 72Ge, 73Ge,74Ge,76Ge was 99.98; 99.90; 99.93 and 87.5 at. substance for separation of germanium isotopes since fluorine is a natural monoisotopic element. GeF is hy- %, respectively, and the content of the impurities of stable 4 drolyzed with water to extract germanium from isotopi- elements was less than 10−5 –10−6 mass %. cally enriched germanium tetrafluoride. The formed fine dispersed residue of germanium dioxide is separated by filtration, dried and reduced with hydrogen up to ele- mental germanium. It is a multi-stage process; germa- 1 Introduction nium tetrafluoride and the products of its hydrolysis are highly corrosive, fine dispersed powders GeO and Ge A stable interest to the isotopic effect in properties of 2 have a developed surface. It leads to contamination of crystalline solid [1–4] made actual the materials science the produced germanium. Its chemical purity can be task of production of single crystals of elemental semi- increased by additional purification by the methods of conductors with high isotopic and chemical purity (sil- fractional recrystallization or zone melting. However, in icon, germanium, selenium, tellurium). Germanium is the process a substantial amount of tail fractions, en- one of promising substances for these investigations. riched with impurities, is formed decreasing the yield of A principal possibility to produce germanium in the the target product. To increase the yield, the tail parts form of perfect single crystals with high chemical pu- of ingots should be again converted into volatile com- rity and presence of five stable isotopes: 70Ge (20.57%), pound and return to technological cycle. This approach 72Ge (27.45%), 73Ge (7.75%), 74Ge (36.50%), 76Ge (7.73%) is suitable for large-scale production but ineffective for [5] makes it a suitable object for acquiring fundamen- tal knowledge on the effect of isotopic composition on properties of semiconductors. High-purity germanium ∗ Corresponding author: e-mail [email protected], Phone: +7831 with natural isotopic composition refers to main materi- 4627650 als used for production of the elements of IR-optics, de- 1 G.G. Devyatykh Institute of Chemistry of High-Purity Substances tectors of ionizing radiation, photodetectors, and precise of RAS, Tropinina str.,49, 603951, Nizhnii Novgorod, Russia temperature sensors. Feasibility of using germanium in 2 Leibniz Institute of Crystal Growth, Max-Born str.,2, 12489, Berlin, photonics, nanoelectronics, spintronics and instruments Germany C 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim (1 of 6) 1700026 M. F. Churbanov et al.: Production of germanium stable isotopes single crystals production of small amounts of high-purity monoiso- and it provides an efficient separation of germanium topic germanium. isotopes by centrifugal method. Monogermane does not In [9] the samples of 70Ge and 74Ge with the content react with main structural materials. Elemental germa- of the main isotope 96% were prepared by fluoride nium can be extracted from monogermane by pyrolysis technology. GeF4 enriched with the target isotope was without application of the methods of «wet» chemistry. Original Paper transformed into GeO2 followed by its reduction to the That is why the hydride method is promising for produc- elemental germanium powder. The Ge crystal grown tion of stable isotopes of germanium with high degree from this material exhibited metallic electrical con- of chemical and isotopic purity. Earlier this method was duction (net carrier concentration > 3 ·1017 cm−3). It developed for production of high purity (net carrier con- was required to develop a special technique for zone centration 1010 cm−3) Ge with natural isotopic composi- purification of germanium to provide decrease of their tion for X-rays detectors [16]. The aim of the present work concentration down to 1012 cm3. 100 g of germanium was the development of completely hydride method for powder was used as a starting material for zone pu- production of stable isotopes of germanium and pro- rification. Then zone refined germanium was used for duction of high-purity single crystals 72Ge, 73Ge,74Ge, crystal growth. Pure single crystals of 70Ge and 74Ge with 76Ge. a weight 4 g was fabricated from 100 g enriched germa- nium powder. It is reported in [10] on preparation of 70Ge sample with the content of the main isotope of 99.99% 2 Experimental by fluoride method. No data are given on the yield of pure monoisotopic germanium. In [11] fluoride method The general scheme of the process included the separa- 76 was developed for production of high-purity Ge for tion of germanium isotopes using monogermane GeH4 detectors in GERDA project. Single crystals (20 kg) as the initial volatile substance, its ultra purification by with purity 12 N was prepared with mass yield 53,3%. the method of low-temperature rectification, extraction This value of yield was achieved by recycling tail parts of germanium by thermal decomposition of monoger- of ingots and scraps to chemical purification. In [12–14] mane, purification of germanium by the method of zone a method is developed for production of isotopically melting, fabrication of single crystalline seed and growth enriched germanium by direct hydrogen reduction of of single crystals. GeF4 in plasma. Germanium was produced in the form of «flakes» which then were melted and the crystal was grown by Czochralski method. Analysis of «flakes» by 2.1 Separation of isotopes SIMS method indicated high content of carbon and oxy- gen (1018–1020 cm−3). 74Ge sigle crystal grown from the Separation of germanium isotopes was carried out «flakes» exhibited electrical resistivity 1,9 Ohm cm and by centrifugal method in OJSC «PO «Electrochemical net carrier concentration 9·1014 cm−3.Thenetcarrier plant»». The initial monogermane with natural isotopic concentration in initial (pure) part of 72Ge sigle crystal af- composition was produced by reaction between germa- ter 4 steps of crystal growth was equal 3,5·1012 cm−3 [12]. nium tetrachloride and sodium-boron hydride. It was In [13] 72Ge sigle crystal, grown from the «flakes» exhib- shown that monogermane does not decompose during ited electrical resistivity 0,8 Ohm cm. Further it was pu- ultra centrifugal process, does not produce noticeable rificated by zone melting and single crystal was prepared corrosive effect on structural materials of separat- from pure part of zone refined ingot. The net carrier con- ing equipment. The attained extraction coefficient of centration in initial (pure) part of crystal was < 1·1013 germanium isotopes was 99 % [17]. cm−3, electrical resistivity - 47 Ohm cm. Insufficient pu- rity of the previously prepared samples of monoisotopic varieties of germanium constraints the work on in-depth 2.2 Ultrapurification of monogermanes investigation of their properties. That is why the fur- ther development of the methods for production of Ge After the stage of separation of isotopes the monoger- isotopes with high chemical and isotopic purity is still manewaspurifiedbythemethodoflow-temperature current. rectification [18]. Ultrapurification of monoisotopic It was shown in [15] that monogermane GeH4 can be monogermanes was carried out by the method of low- used as a volatile compound for separation of germa- temperature batch rectification in packed column with nium isotopes. Natural hydrogen is actually of monoiso- middle still at –85 оС and pressure of 1.5 bar (abs.) topic nature (the content of 1H isotope is 99.985 at. %) Rectifying sections with height of 40 and 70 cm and cross 1700026 (2 of 6) C 2017WILEY-VCHVerlagGmbH&Co.KGaA,Weinheim www.crt-journal.org Cryst. Res. Technol., 1700026 (2017) section of 2 cm2 are filled with spiral prismatic packing from nichrome wire 2.5 × 2.5 × 0.2 mm. To prevent iso- topic dilution, the column was flushed out from traces of monogermane of another isotopic composition using a specially developed technique. Sampling of fractions, enriched with lower- (light fraction) and higher-boiling Original Paper (heavy fraction) impurities was simultaneously con- Fig. 1 Growth of single crystal of monoisotopic germanium in 2 ducted from top and bottom of the column in discrete stages.
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