High purity hafnium, target and thin film comprising said high purity hafnium, and method for producing high purity hafnium
a technology of high purity hafnium and target, which is applied in the direction of vacuum evaporation coating, coating, sputtering coating, etc., can solve the problems of unstable required characteristics of hafnium raw materials, inability to efficiently eliminate, and inability to efficiently obtain the foregoing high purity hafnium material. , to achieve the effect of high purity, stably manufacturing high purity hafnium, and superior
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example 1
[0029] 100 Kg of commercially available hafnium tetrachloride (HfCl4) shown in Table 1 having a purity of 3N and containing roughly 5000 wtppm of zirconium was used as the raw material, and this was dissolved in 1 L of purified water to create a nitric acid solution.
[0030] This raw material contained 500 wtppm, 40 wtppm and 1000 wtppm of iron, chrome and nickel, respectively, as its main impurities in HfCl4.
[0031] Next, this hafnium raw material (a nitric acid solution) was subject to 4-stage organic solvent extraction using a TBP organic solvent, and neutralization treatment was performed to obtain hafnium oxide (HfO2).
[0032] Further, this hafnium oxide was subject to chlorination to obtain high purity hafnium tetrachloride (HfCl4), and then subject to magnesium reduction to obtain a hafnium sponge as the raw material. This hafnium sponge contained 300 wtppm of zirconium, and the total content of other impurities was reduced to 300 wtppm.
[0033] Next, the obtained hafnium sponge...
example 2
[0037] 100 Kg of hafnium metal raw material (zirconium content of 2 wt %) shown in Table 2 was used and dissolved in nitric-hydrofluoric acid. This raw material contained 15000 wtppm, 8000 wtppm and 5000 wtppm of iron, chrome and nickel, respectively, as its main impurities in the raw material.
[0038] Next, this hafnium raw material was subject to 10-stage organic solvent extraction using a TBP organic solvent, and neutralization treatment was performed to obtain hafnium oxide (HfO2).
[0039] Further, this hafnium oxide was subject to chlorination to obtain high purity hafnium tetrachloride (HfCl4), and then subject to calcium reduction to obtain a hafnium sponge. This hafnium sponge contained 1500 wtppm of zirconium, and the total content of other impurities was reduced to 1000 wtppm.
[0040] Next, the obtained hafnium sponge was used as the raw material, and further subject to two-stage melting via hearth melting and ingot melting with an electron beam to remove volatile elements, g...
example 3
[0043] 100 Kg of hafnium oxide (HfO2) raw material (3N level) shown in Table 3 was used and dissolved in nitric-hydrofluoric acid. This raw material contained 15000 wtppm, 8000 wtppm and 5000 wtppm of iron, chrome and nickel, respectively, as its main impurities in the raw material.
[0044] Next, this hafnium oxide raw material was chlorinated and subject to refining with distillation of 10 or more stages, then further subject to sodium reduction.
[0045] Next, the obtained hafnium was used as the raw material, and further subject to two-stage melting via hearth melting and ingot melting with an electron beam to remove volatile elements, gas components and so on. As a result of the foregoing process, as shown in Table 3, realized was Zr: 500 wtppm, O: 100 wtppm, C: 100 wtppm, N: 20 wtppm, S: 10 wtppm, P: 10 wtppm, others: 30 wtppm.
[0046] Next, the hafnium thus obtained was subject to deoxidation at 1250° C., under argon pressure (4 atm) for 10 hours with molten salt of Ca and CaCl2. ...
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