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The inherent properties of metals are affected by impurity elements, sometimes strongly. There are many brittle phenomena in iron and its alloys due to the harmful effect of trace impurities such as sulphur, phosphorus, hydrogen and so on. On the other hand, a large number of alloying elements also embrittle iron due to the transformation and precipitation of secondary phase. For example, the ductility of Fe-Cr alloy decreases with the increase in chromium content, although the strength and the corrosion resistance increase with chromium content. In Fe-Cr alloy containing high chromium, 475°C embrittlement and σ-phase embrittlement are well known. An Fe-50mass%Cr alloy of conventional purity is extremely brittle due to the formation of σ-phase. However, we found the highly purified alloy is essentially ductile. In the workshop of UHPM-94, the experimental results on the ductility of Fe-50mass%Cr alloy were presented and discussed. In this research, the effect of purification on the hot ductility of high purity Fe-18mass%Cr and Fe-50mass%Cr alloys was investigated by tensile testing at high temperature. It was found that the ductility of Fe-18mass%Cr alloy is remarkably improved by purification, especially by the reduction of interstitial impurities such as carbon and nitrogen. The highly-purified Fe-50mass%Cr alloy has astonishing ductility at the temperature range between room temperature and 1073K. Also in a high purity Fe-50mass%Cr alloy, the formation of the σ-phase was not observed during ageing for 1000h at 973K. These results are also very important for the development of high-performance Fe-Cr alloys and of the manufacturing process. Consequently, purification technology is very useful for progress in metal science.

Stress Corrosion Cracking (SCC) sensitivities of high purity Fe-Cr alloys were investigated in simulated Boiling Water Reactor (BWR) and primary Pressurized Water Reactor (PWR) cooling waters, by constant extension rate tests (CERT) at a strain rate of 4x10-7s-1. No high purity Fe-Cr alloy showed any SCC sensitivity in either simulated BWR and PWR primary water environment.

Fe-50mass%Cr was prepared in a cold crucible furnace with induction heating, then refined by floating-zone melting (FZM). The chemistries on the surface before and after FZM were compared by XPS measurement. C and O were observed on top surfaces both before and after as a hydrocarbon, carbonyl group and carboxyl group which are adsorbed chemical components. The other impurities were observed on the surface in both cases ; however, the number and level of impurities on the surface after FZM were much larger than those on the surface before FZM ; these adhered to the surface during sample preparation for XPS measurement. It is concluded that sample preparation introduces contamination which affects the detection limit of chemical analytical instruments. Sn was only observed on the top surface after FZM. It was segregated Sn which was contained in chromium as a starting material. It must be eliminated before starting. From XPS depth profiling results, it was concluded that 0.2 nm thickness of carbon such as hydrocarbon and organic components are adsorbed on the 1 nm thickness of oxide layer. Below the oxide layer, a lack of Cr was observed down to a depth of 6 nm.

Radiation-induced precipitates on dislocation loops in low and high purity Fe-9, -18 and -50 % Cr alloys were examined under electron irradiation in a high voltage electron microscope operated at 1 MV. Two types of dislocation loops on {100} planes with a <100> Burgers vectors and on {111} planes with a /2<111> are formed in high purity Fe-Cr alloys. However, only a <100> type loops are formed in low purity alloys, i.e. where carbon concentration is greater than about 60 wt.ppm. The growth rate of the loops formed in Fe-9 and -18Cr alloys is faster than that of Fe-50Cr alloy. All of the loops formed at temperatures ranging from 573 K to 973 K, even in the ( σ+α+α') phase regions in thermal equilibrium, have moiré fringe contrast due to precipitates identified as α' phase. The contrast is very weak in the Fe-50Cr alloy because of coarse distribution of precipitates, while the α' phase formed in low purity alloys has somewhat larger interplanar spacings that are modified by interstitial impurities. The α' phase formation on the loops can be understood by radiation-induced segregation of chromium and interstitial impurity atoms.

High purity Fe-50mass%Cr alloys containing (C+N) in the range of 30 to 500 mass ppm were prepared and their corrosion resistance was investigated. Pitting potential in a 3.5mass%NaCl solution at 343K rose with reducing (C+N) content. Alloys containing (C+N) at less than 100 mass ppm did not sustain pitting corrosion. However, alloys containing 500 mass ppm (C+N) corroded severely in 6%FeCl3+1/20N HCl solutions. Heat treatment at 923K was recognized as influencing corrosion resistance due to precipitation of carbonitrides only in the case of the alloy containing 500 mass ppm (C+N).

Tensile tests on high purity Fe-P alloys with 0, 0.05 and 0.1 mass%P were carried out at temperatures between 300 K and 1073 K to clarify the intrinsic effect of phosphorus on the mechanical properties of iron at elevated temperatures. Microstructures of as-quenched, interrupted and ruptured specimens were observed. Experimental results show that the addition of phosphorus causes a remarkable increase in proof stress of high purity iron at 300 K, but the increase in proof stress by phosphorus decreases with increasing test temperature. The strengthening effect of phosphorus reduces to zero at 1073 K. High purity iron and Fe-P alloys rupture at almost 100% reduction in area at the whole test temperatures. However, Fe-P alloys show much larger elongation at test temperatures above 773 K than high purity iron. The increased elongation of high purity iron by addition of phosphorus was shown to be related to the effect of phosphorus on dynamic recovery and recrystallization of iron as its intrinsic effect.

A new induction heating floating-zone refining (IHFZR) furnace was designed and constructed using ultrahigh vacuum technology for the ultrapurification of base metals. The ultrahigh vacuum attainable in this furnace is so good as 1x10-7}Pa that a base metal bar can be zone-melted in both ultrahigh vacuum and higher-purity gas atmosphere containing less residual gases. The outline of this IHFZR furnace and the results of its application to the purification of high-purity iron, Fe-18%Cr alloy and Fe-50%Cr alloy are described. After only two zone-leveling passes in dry hydrogen, oxygen easily decreases in concentration from over 60 mass ppm to a few mass ppm ; on the other hand, carbon decreases in concentration not so easily as oxygen but gradually. As a result, ultrahigh-purity Fe-18%Cr alloy with the concentration of C+N+O+S of 12 mass ppm and ultrahigh-purity Fe-50%Cr alloy with the concentration of C+N+O+S of 10 mass ppm were obtained after only two zone-leveling passes and ten zone-leveling passes in dry hydrogen, respectively.

The ductility of ultra-high purity copper at elevated temperatures was investigated : purity 99.9999% (6N) and 99.999999% (8N). Tensile tests were conducted at temperatures ranging from 293K to 1073K at strain rates of 4.2x10-5s-1in a high vacuum. The results are discussed in comparison with those for 99.9% (3N) copper. Ductility at intermediate temperatures was improved by an increase in purity. The temperature at which ductility dropped decreased with increases in purity. Even at the ultra-high purity of 8N, a small ductility drop was observed at 423K. A small number of micro voids were observed on the grain boundaries of 8N specimens after the test at 423K. 6N and 8N copper have nearly same sulphur content of about 0.015 ppm. The intermediate temperature embrittlement of these coppers might be affected not only by sulphur content, but also by total impurity content.