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Ultra-Purification of Electrolytic Iron by Cold-Crucible Induction Melting

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Ultra-Purification of Electrolytic Iron by Cold-Crucible Induction Melting Materials Transactions, JIM, Vol. 41, No. 1 (2000) pp. 2 to 6 Special Issue on Ultra-High Purity Metals c 2000 The Japan Institute of Metals Ultra-Purification of Electrolytic Iron by Cold-Crucible Induction Melting and Induction-Heating Floating-Zone Melting in Ultra-High Vacuum Seiichi Takaki and Kenji Abiko Institute for Materials Research, Tohoku University, Sendai 980-8577, Japan The effect of melting under ultra-high vacuum of 10¡7 Pa on the purification of the high-purity electrolytic iron developed was investigated using a new cold-crucible induction melting furnace which was able to melt high-purity iron of 10 kg and a new induction-heating floating-zone melting furnace, which were designed and constructed using ultra-high vacuum technology. Ultra-high vacuum melting was quite useful even for the ultra-purification of iron 10 kg in weight. The high-purity electrolytic iron of 7.5 kg with residual resistivity ratio of 2000 to 2700 was melted using the cold-crucible induction melting furnace, and the pressure during melting after melt-down was kept from 1 £ 10¡6 to 8 £ 10¡7 Pa for 9 min. The 7.5 kg ultra-pure iron ingot of more than 99.9988 mass% purity after the chemical analysis of 33 elements, most of which were lower than each detection limit, was successfully obtained, even if this ingot contains their all elements of the detection limit value. Also the ultra-pure iron 35 g in weight of more than 99.9988 mass% purity was obtained from electrolytic iron of 99.996 mass% purity by the combination of cold-crucible induction melting in ultra-high vacuum and induction-heating floating-zone melting in UHV of 4 £ 10¡7 Pa after the analysis of 35 elements. The concentration of C C N C O C S decreases from 14.4 mass ppm before zone-leveling to 2.4 mass ppm after four zone-leveling passes in ultra-high vacuum. For further ultra-purification of iron it is absolutely necessary to develop and establish the trace analysis techniques of measuring accurately the concentration of non-metallic impurity elements at levels below 0.1 mass ppm and metallic impurity elements at levels below 0.01 or 0.001 mass ppm. (Received January 12, 2000) Keywords: high-purity electrolytic iron, ultra-high purity iron, ultra-purification, ultra-high vacuum, cold-crucible induction-melting, induction-heating floating-zone melting, electron-beam floating-zone melting, trace analysis Ref. 6). 1. Introduction The purpose of the present work is to investigate the effect of melting under ultra-high vacuum of 10¡7 Pa on the purifi- For the fundamental research on the intrinsic properties of cation of the high-purity electrolytic iron as follows and to es- iron and also to determine the inherent effects of each impu- tablish a new purification procedure to obtain ultra-pure iron: rity element on the properties ultra-high purity iron is essen- (1) two kinds of electrolytic iron about 10 kg in weight are tial. There have been many studies of the purification of iron melted under UHV of 10¡7 Pa in CCIM furnace and (2) the in the literature,1) but few which describe the effect of ultra- iron bars less than 50 g in weight prepared from iron ingot ob- high vacuum (UHV) on it, because it is not easy to attain to tained by CCIM in UHV of 10¡6 Pa are further zone-melted ultra-high vacuum better than 1 £ 10¡6 Pa during melting of in UHV of 10¡7 Pa using the IHFZM furnace. The UHV at- iron in a large melting furnace. tainable in both our CCIM and IHFZM furnaces is better than We previously reported2) that ultra-high purity iron 15 g 1 £ 10¡7 Pa. in weight with the residual resistivity ratio (RRRHD64 kA/m) of more than 5000 was prepared by electron-beam floating- 2. Experimental Procedure zone melting (EBFZM) under an ultra-high vacuum of the order of 10¡7 Pa using Johnson-Matthey pure iron as start- 2.1 Starting materials ing iron bars. The production of high-purity electrolytic iron Two kinds of electrolytic iron (EFe) developed by us,3) has been developed by us3) and the purity attainable is in- high-purity iron and higher-purity iron were used as the creasing year by year. On the other hand, we have made starting materials. The analytical results of two batches of surface analysis experiments on Fe–P alloys under an ultra- high-purity electrolytic iron, EFe-1 and EFe-2, are shown in high vacuum of 4 £ 10¡9 Pa.4) We also designed and made Table 1. The purity was more than 99.996 mass% after the a new high-temperature optical microscope using UHV tech- analysis of 35 elements. For the higher-purity electrolytic nology.5) Then, on the basis of such our experience and the iron, EFe-3, not chemical analysis but residual resistivity ratio background mentioned above, we started to design and build (RRRH ) measurement was performed and the RRRH value new purification apparatus to prepare ultra-high purity base was from 2000 to 2700 for 16 batchs of higher-purity elec- metal specimens, and first in UHPM-94 we reported on the trolytic iron. construction of a new arc melting furnace by using UHV tech- nology,6) second in UHPM-95 on the construction of a new 2.2 Cold-crucible induction melting induction-heating floating-zone melting (IHFZM) furnace7) The new induction melting furnace with a cold-copper cru- and then on the construction of a new cold-crucible induction- cible is described in detail in Ref. 8). This furnace can melting (CCIM) furnace8) in UHPM-97 and a part of the re- make an iron ingot up to 10 kg. The power supply provides sults of the purification effect by CCIM.9,10) The importance max. 240 kW and 10 kHz. The main chamber which has two of UHV in a purification apparatus is described in detail in flanges of 1.4 m in diameter and a volume of about 2.3 m3 can Ultra-Purification of Electrolytic Iron by Cold-Crucible Induction Melting and Induction-Heating Floating-Zone Melting in Ultra-High Vacuum 3 Table 1 Results of chemical analysis of iron samples (mass ppm). Starting iron Iron ingot IFe-1 IFe-2 IFe-3 EFe-1 EFe-2 EFe-1CEFe-2 EFe-1CEFe-2 EFe-3 CCIM, >4 £ 10¡6 Pa CCIM, >2 £ 10¡6 Pa CCIM, >8 £ 10¡7 Pa C 3.2 3.5 1.0 0.7 0.6 N <0.1 0.1 <0.1 0.8 <0.1 O 24 12 7.2 6.0 1.9 S 1.3 1.1 0.5 0.7 0.8 H 1.3 1.0 0.7 ----------------------------------------------------------------------- Al 3.1 <0.2 0.2 <0.4 <0.4 As 1.2 0.8 1.1 1.6 1.4 B 0.6 0.3 0.03 0.38 0.12 Ba <0.1 <0.1 <0.1 <0.1 <0.1 Bi <0.1 <0.1 <0.1 <0.1 <0.1 Ca <0.2 <0.2 <0.2 Cd <0.001 <0.001 <0.001 <0.001 <0.001 Co 0.3 <0.1 0.7 <0.1 0.6 Cr <0.3 <0.3 0.2 0.5 <0.5 Cu 0.4 0.2 0.5 0.2 0.2 Ga <0.2 0.3 0.2 <0.3 <0.3 Hf <0.06 <0.06 <0.06 <0.07 <0.07 Mg <0.01 <0.01 <0.01 <0.02 <0.02 Mn <0.01 <0.01 <0.01 <0.01 <0.01 Mo 0.1 <0.1 0.1 <0.3 <0.3 Nb <0.05 <0.05 <0.05 <0.03 <0.04 Ni <0.1 0.1 0.1 <0.1 0.2 P 0.1 0.7 0.1 0.3 0.3 Pb <0.01 0.12 0.04 <0.03 <0.03 Sb <0.3 <0.3 <0.3 <0.3 <0.3 Se <0.04 <0.04 <0.04 <0.04 <0.04 Si11111 Sn <0.4 <0.4 <0.4 <0.5 <0.5 Ta <0.6 <0.6 <0.6 <0.9 <0.9 Te <0.03 <0.03 <0.03 <0.02 <0.02 Ti <0.2 <0.2 <0.1 <0.2 <0.2 V 0.03 0.03 0.05 <0.03 <0.03 W <1 <1 <111 Zn 1.6 14.2 0.6 <0.1 <0.1 Zr <0.2 <0.2 0.2 <0.07 <0.07 Purity >99.996% >99.996% >99.9982% >99.9983% >99.9988% be evacuated to a base pressure of 6:7 £ 10¡8 Pa by a system flow of high-purity hydrogen or in UHV. The UHV attainable of an oil diffusion pump and a cold trap. The total pressure in this IHFZM furnace is better than 1 £ 10¡7 Pa. An exam- and the partial pressure of mass number between 1 and 50 ple of the vacuum during each zone-leveling pass in UHV is in the main chamber were measured before, during and after shown in Table 3. The zone travel rate was 2.5 mm/min and melting as seen below. the distance was about 90 mm for FZM only in UHV, about The ingot obtained was heated in high-purity Ar atmo- 120 mm for FZM only in hydrogen and about 55 mm for FZM sphere at 1150 K and then forged, rolled and machined to rods in hydrogen and then in UHV.
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