US20020117022A1 - High purity iron, method of manufacturing thereof, and high purity iron targets - Google Patents

High purity iron, method of manufacturing thereof, and high purity iron targets Download PDF

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US20020117022A1
US20020117022A1 US09/966,425 US96642501A US2002117022A1 US 20020117022 A1 US20020117022 A1 US 20020117022A1 US 96642501 A US96642501 A US 96642501A US 2002117022 A1 US2002117022 A1 US 2002117022A1
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Prior art keywords
iron
aqueous solution
ions
high purity
copper
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Masahito Uchikoshi
Norio Yokoyama
Tamas Kekesi
Minoru Isshiki
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Sony Corp
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Sony Corp
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Assigned to SONY CORPORATION reassignment SONY CORPORATION ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: ISSHIKI, MINORU, KEKESI, TAMAS, UCHIKOSHI, MASAHITO, YOKOYAMA, NORIO
Publication of US20020117022A1 publication Critical patent/US20020117022A1/en
Priority to US10/446,427 priority Critical patent/US20030206822A1/en
Abandoned legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/16—Remelting metals
    • C22B9/22—Remelting metals with heating by wave energy or particle radiation
    • C22B9/226—Remelting metals with heating by wave energy or particle radiation by electric discharge, e.g. plasma
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • the present invention relates to high purity iron in which contents of impurities such as copper are reduced, a method of manufacturing thereof, and high purity iron targets.
  • VLSI very large scale integrated circuit
  • ULSI ultra LSI
  • Si silicon
  • Fe iron
  • MRAM magnetic random access memory
  • Cu copper
  • U uranium
  • Th thorium
  • iron silicide FeSi 2
  • FeSi 2 iron silicide
  • GaAs gallium arsenide
  • CdTe cadmium telluride
  • the upper limit of impurity content in iron silicide is less than in substances of semiconductor devices of VLSI and ULSI. Small amounts of impurities form impurity level that causes degradation of the semiconductor properties.
  • iron as a semiconductor material needs high purity.
  • the floating zone melting refining method is intended to further raise the purity levels of metals purified to some extent, and in practice, it is reported that the floating zone melting refining method has large effects on purification (Yukio Ishikawa, Koji Mimura, Minoru Isshiki, Bulletin of the Institute for Advanced Materials Processing Tohoku University 51 (1995), pp.10-18).
  • it is difficult to apply the floating zone melting refining method to large scale and the method may not always produce high purity metals surely, that is, it is difficult to produce a large amount of high purity iron at a low price with the floating zone melting refining method. Therefore, a need exists for methods of purifying iron easily, surely, and highly, and particularly for the development of methods of removing copper.
  • the present invention has been achieved in view of the above problems. It is an object of the invention to provide high purity iron and high purity iron targets in which contents of impurities such as copper are reduced.
  • the invention provides high purity iron with 99.99 mass % or more in purity wherein a copper impurity content is 50 mass ppb or less.
  • the invention provides high purity iron wherein a residual resistivity ratio thereof is 3000 or more, and a copper impurity content is 50 mass ppb or less.
  • a method of manufacturing high purity iron according to the invention comprises the steps of; converting trivalent iron ions and impurity divalent copper ions contained in an aqueous solution of iron chloride respectively to divalent iron ions and monovalent copper ions; adjusting a concentration of hydrochloric acid in a range of 0.1 kmol/m 3 to 6 kmol/m 3 ; and separating the monovalent copper ions from the aqueous solution of iron chloride by using the ion exchange resins.
  • a method of manufacturing high purity iron comprises: converting trivalent iron ions in an aqueous solution of iron chloride to divalent iron ions; adjusting a concentration of hydrochloric acid in a range of 0.1 kmol/m 3 to 6 kmol/m 3 ; and separating impurities of at least one selected from the group consisting of zinc, gallium, niobium, technetium, ruthenium, rhodium, palladium, silver, cadmium, indium, tin, antimony, tellurium, tantalum, tungsten, rbenium, osmium, iridium, platinum, gold, mercury, thallium, lead, and bismuth from the aqueous solution of iron chloride by using the anion exchange resins.
  • the invention provides high purity iron targets with 99.99 mass % or more in purity wherein a copper impurity content is 50 mass ppb or less.
  • the invention provides high purity iron targets wherein a residual resistivity ratio is 3000 or more, and a copper impurity content is 50 mass ppb or less.
  • a concentration of copper is reduced to 50 mass ppb or less to achieve high purification.
  • the method of manufacturing the high purity iron according to the invention includes the steps of converting trivalent iron ions and divalent copper ions respectively to divalent iron ions and monovalent copper ions, and adjusting a concentration of hydrochloric acid. These steps allow monovalent copper ions to be absorbed on the anion exchange resins, and divalent iron ions not to be absorbed thereon. Thus the copper can be separated easily and surely from the aqueous solution of iron chloride.
  • Another method of manufacturing high purity iron includes the steps of converting trivalent iron ions in an aqueous solution of iron chloride to divalent iron ions and adjusting a concentration of hydrochloric acid. These steps allow at least one of impurities selected from the group consisting of zinc, gallium, niobium, technetium, ruthenium, rhodium, palladium, silver, cadmium, indium, tin, antimony, tellurium, tantalum, tungsten, rhenium, osmium, iridium, platinum, gold, mercury, thallium, lead, and bismuth to be absorbed on the anion exchange resins, and divalent iron ions not to be absorbed thereon.
  • impurities can be separated easily and surely from the aqueous solution of iron chloride.
  • FIG. 1 is a flow chart illustrating a manufacturing process of high purity iron and high purity iron targets according to one embodiment of the invention.
  • FIG. 2 is a flow chart illustrating the manufacturing process following FIG. 1.
  • FIG. 3 is a diagram explaining one step of the manufacturing process shown in FIG. 1.
  • FIG. 4 is a diagram explaining another step of the manufacturing processes shown in FIG. 1.
  • FIG. 5 is a graph illustrating changes of the concentrations of metal ions in the effluent of the anion exchange resins.
  • FIG. 6 is another graph illustrating changes of the concentrations of metal ions in the effluent of the anion exchange resins.
  • high purity iron and high purity iron targets have 99.99 mass % or more in purity, preferably 99.999 mass % or more, or the residual resistivity ratios thereof are 3000 or more and copper impurity content thereof is 50 mass ppb or less.
  • the term “purity” (namely, chemical purity) used herein means values obtained by one minus all concentrations of impurities possible to be determined by using present analysis apparatus and methods (Minoru Isshiki, Koji Mimura, Bulletin of the Japan Institute of Metals, 31 (1992), 880-887). For example, the values can be obtained by one minus the concentrations of impurities of 70 or more elements determined by Glow Discharge Mass Spectroscopy.
  • concentrations of gas elements such as oxygen, nitrogen, and hydrogen, if required, can be determined by appropriate methods such as a non-dispersive infrared absorption method, a thermal conductivity method, and a heat conduction measurement of such gas elements separated with a column after being fused in an inert gas.
  • residual resistivity ratios provide one index showing purities of highly purified metals, and as shown in the formula I, the residual resistivity ratio is the ratio of resistivity at 298K to resistivity at 4.2K.
  • the formula II shows a relationship between resistivity and resistance (electric resistance). Therefore, the formula I expressing the residual resistivity ratio can be transformed into the formula III, and if volume. changes by temperature are negligible, the formula I can be approximated by the ratio of the resistance at 298K to the resistance at 4.2K.
  • iron is a ferromagnetic metal and factors such as geomagnetism, demagnetization conditions, and magnetic fields by measurement currents can affect the resistance measurements. Thus, it is necessary to apply vertical magnetic field that is preferably about 60 kA/m in measuring the resistance in order to suppress these influences (Seiichi Takagi, Materia Japan, 33 (1994), 6-10).
  • R 298K , S 298K , and L 298K respectively, resistance, cross-section area, length at 298K
  • R 4.2K , S 4.2K , and L 4.2K respectively resistance, cross-section area, length at 4.2K
  • the high purity iron and the high purity iron targets may be used as materials of devices, for example, semiconductor devices, magnetic recording mediums, magnetic recording heads, and devices with environmental semiconductors.
  • the term “environmental semiconductor” used herein means a semiconductor substance that exists abundantly on the earth and consists of an eco-friendly material, for example, iron silicide (FeSi 2 ) and calcium silicide (Ca 2 Si) (See the website of Society of Kankyo Semiconductors (http://kan.engjm.saitama-u.ac.jp/SKS/index 2 .html)).
  • Such high purity iron and such high purity iron targets can be manufactured as follows.
  • FIGS. 1 and 2 show the manufacturing process of the high purity iron according to the embodiment.
  • the iron containing impurities such as copper is dissolved in a hydrochloric acid solution in order to prepare an aqueous solution of iron chloride (FeCl 2 or FeCl 3 ) (Step S 101 ).
  • the concentration of the hydrochloric acid is adjusted in a range of 0.1 kmol/m 3 to 6 kmol/m 3 .
  • the aqueous solution of iron chloride M is poured into a container 12 with a metal 11 such as iron. Then, the aqueous solution of iron chloride M is sufficiently contacted with the metal 11 by agitating with a device such as a stirrer 14 , while injecting an inert gas 13 such as nitrogen gas (N 2 ) or argon gas (Ar) into the aqueous solution of iron chloride M (Step S 102 ).
  • an inert gas 13 such as nitrogen gas (N 2 ) or argon gas (Ar)
  • the copper contained in the aqueous solution of iron chloride M will react with the metal 11 , for example, as shown in the following chemical formula 1, converting the divalent copper ions to monovalent copper ions or metallic copper.
  • the iron contained in the aqueous solution of iron chloride M will react with the metal 11 , for example, as shown in the following chemical formula 2, converting the trivalent iron ions to divalent iron ions. It should be noted that the reaction of the chemical formula 1 may not completely proceed to the right-hand side and a small amount of the monovalent copper ions may remain in the aqueous solution of iron chloride.
  • Dissolved oxygen can prevent reactions such as the above chemical formulas 1 and 2. Therefore, injecting the inert gas 13 into the aqueous solution of iron chloride M intends to remove oxygen dissolved in the aqueous solution of iron chloride M, in order to carry out the reactions.
  • the inert gas 13 may be injected with agitating the aqueous solution of iron chloride M containing the metal 11 , or before the metal 11 is added into the aqueous solution of iron chloride M.
  • the metal 11 has large surface area such as powder, which can contact more effectively with the aqueous solution of iron chloride M and react sufficiently with the copper ions and iron ions.
  • Substances other than iron can also be used for the metal 11 . It is preferred to use iron for the metal 11 in order to avoid other impurities from contaminating the aqueous solution of iron chloride M as much as possible.
  • the trivalent iron ions and divalent copper ions in the aqueous solution of iron chloride M may be converted respectively to the divalent iron ions and the monovalent copper ions by contacting with the metal 11 after adjusting the concentration of hydrochloric acid in the aqueous solution of iron chloride M as described above, or before adjusting the concentration of hydrochloric acid in the aqueous solution of iron chloride.
  • a column 22 is filled up with the anion exchange resins 21 , the aqueous solution of iron chloride M is fed into the column 22 from a storage tank 23 , and is contacted with the anion exchange resins 21 sufficiently (Step S 103 ).
  • the flow rate of the aqueous solution of iron chloride M is determined effectively to contact the aqueous solution of iron chloride M with the anion exchange resins 21 sufficiently, and is preferably 1 bed volume(s)/hour.
  • FIG. 5 shows changes of the concentrations of metal ions in the effluent (elution curve).
  • the abscissa represents the effluent volumes and the ordinate represents the concentrations standardized by the maximum concentrations of the metal ions.
  • impurities selected from the group consisting of zinc (Zn), gallium (Ga), niobium (Nb), technetium (Tc), ruthenium (Ru), rhodium (Rh), palladium (Pd), silver (Ag), cadmium (Cd), indium (In), tin (Sn), antimony (Sb), tellurium (Te), tantalum (Ta), tungsten (W), rhenium (Re), osmium (Os), iridium (Ir), platinum (Pt), gold (Au), mercury (Hg), thallium (Tl), lead (Pb), and bismuth (Bi) is contained in the aqueous solution of iron chloride M, as well as zinc and tin as shown in FIG. 5, in the Step S 103 , these impurities can be absorbed on the anion exchange resins 21 with monovalent copper ions and can be also separated from the aqueous solution of iron chloride M, as well as zinc and
  • the concentration of hydrochloric acid of aqueous solution of iron chloride M is adjusted in a range of 2 kmol/m 3 to 11 kmol/m 3 and, as shown in FIG. 4, the aqueous solution of iron chloride M is sufficiently contacted with the anion exchange resins 21 (Step S 105 ).
  • the trivalent iron ions will be absorbed on the anion exchange resins 21 , and the impurities such as lithium, beryllium, sodium, magnesium, aluminum, silicon, phosphorus, potassium, calcium, scandium, titanium, vanadium, chromium, manganese, cobalt, nickel, rubidium, strontium, yttrium, zirconium, cesium, barium, lanthanoids, hafnium, francium, radium, and actinoids will not be absorbed on the anion exchange resins 21 and be eluted.
  • the impurities such as lithium, beryllium, sodium, magnesium, aluminum, silicon, phosphorus, potassium, calcium, scandium, titanium, vanadium, chromium, manganese, cobalt, nickel, rubidium, strontium, yttrium, zirconium, cesium, barium, lanthanoids, hafnium, francium, radium, and actinoids will not be absorbed on the anion
  • FIG. 6 shows changes of the concentrations of metal ions in the effluent (elution curve).
  • the changes of the concentrations of some typical impurities that is, aluminum, silicon, phosphorus, titanium, manganese, cobalt, and chromium, are shown in the FIG. 6 for comparison with the iron.
  • the abscissa and the ordinate represent respectively the equivalents in the FIG. 5.
  • there is no range to which the peaks of the elution curves of the trivalent iron ions and these impurities overlap which shows that these impurities can be completely separated from the aqueous solution of iron chloride.
  • impurities selected from the group consisting of zinc, gallium, niobium, molybdenum (Mo), technetium, ruthenium, rhodium, palladium, silver, cadmium, indium, tin, antimony, tellurium, tantalum, tungsten, rhenium, osmium, iridium, platinum, gold, mercury, thallium, lead, bismuth and polonium (Po) is contained in the aqueous solution of iron chloride M, these impurities can be absorbed on the anion exchange resins 21 as well as the iron in the Step S 105 .
  • impurities selected from the group consisting of zinc, gallium, niobium, molybdenum (Mo), technetium, ruthenium, rhodium, palladium, silver, cadmium, indium, tin, antimony, tellurium, tantalum, tungsten, rhenium, osmium,
  • Changes of the concentrations of metal ions in the effluent in the Step S 106 are also shown in the FIG. 6. Especially, in the FIG. 6, the changes of the concentrations of some typical impurities, that is, molybdenum and zinc are shown for comparison with the iron. As shown in FIG. 6, there is no range to which the peaks of the elution curves of the trivalent iron ions and these impurities overlap, which shows that these impurities can be completely separated from the iron.
  • molybdenum and polonium will be mainly separated from the iron in the Step S 106 , because zinc, gallium, niobium, technetium, ruthenium, rhodium, palladium, silver, cadmium, indium, tin, antimony, tellurium, tantalum, tungsten, rhenium, osmium, iridium, platinum, gold, mercury, thallium, lead, and bismuth have already been separated from the aqueous solution of iron chloride M with the copper in the Step S 103 .
  • the obtained aqueous solution of iron chloride M is evaporated to dryness and is oxidized in order to obtain iron oxide (Step S 107 ). Then, the obtained iron oxide is heated from 500 K to less than 1800 K in a hydrogen atmosphere (Step S 108 ). It is preferred to heat to 1000 k or above for rapid reduction. Thus, the iron oxide will react as shown in the following chemical formula 3 to obtain iron.
  • the obtained iron is molten with plasma arc using a plasma generation gas containing active hydrogen, in order to remove at least one of impurities selected from the group consisting of oxygen, nitrogen, carbon (C), sulfur, halogen, alkaline metals, and alkaline-earth metals (Step S 109 ).
  • a plasma generation gas containing active hydrogen in order to remove at least one of impurities selected from the group consisting of oxygen, nitrogen, carbon (C), sulfur, halogen, alkaline metals, and alkaline-earth metals.
  • the contents of copper may be reduced to 50 mass ppb or less. Therefore, the high purity iron or the iron targets according to the invention may not be responsible for short circuit of devices such as semiconductor devices and can be applied to the semiconductor devices for the enhancement of properties. Moreover, the high purity iron and the high purity iron targets can be used for devices such as magnetic recording mediums and magnetic recording heads for the enhancement of properties. In addition, the high purity iron and the high purity iron targets used as materials of compound semiconductors such as iron silicide may not cause unwanted impurity level formed by small amounts of impurities responsible for property degradation and will provide good semiconductor properties.
  • the trivalent iron ions and the divalent copper ions are converted respectively to the divalent iron ions and the monovalent copper ions, the concentration of the hydrochloric acid is adjusted from 0.1 kmol/m 3 to 6 kmol/m 3 , and the aqueous solution of iron chloride is contacted with the anion exchange resins. Therefore, the copper may be separated from the aqueous solution of iron chloride easily and the high purity iron and the high purity iron targets with low concentrations of copper can be obtained easily and surely.
  • converting the trivalent iron ions to the divalent iron ions allows at least one of impurities selected from the group consisting of zinc, gallium, niobium, technetium, ruthenium, rhodium, palladium, silver, cadmium, indium, tin, antimony, tellurium, tantalum, tungsten, rhenium, osmium, iridium, platinum, gold, mercury, thallium, lead, and bismuth to be separated easily from the aqueous solution of iron chloride M as well as the copper.
  • impurities selected from the group consisting of zinc, gallium, niobium, technetium, ruthenium, rhodium, palladium, silver, cadmium, indium, tin, antimony, tellurium, tantalum, tungsten, rhenium, osmium, iridium, platinum, gold, mercury, thallium, lead, and bismuth
  • FIGS. 1 to 6 The invention will be further described in detail by reference to FIGS. 1 to 6 .
  • the same reference numbers and signs will be used for equivalents of the substances in the above embodiments.
  • a hydrogen peroxide solution was added to the aqueous solution of iron chloride M to convert the divalent iron ions to trivalent iron ions (Step S 104 ). Then, the concentration of hydrochloric acid of the aqueous solution of iron chloride M was adjusted to 5 kmol/m 3 , and the aqueous solution of iron chloride M was contacted with the anion exchange resins 21 to absorb the trivalent iron ions and separate impurities such as lithium (Step S 105 ). Then, the iron was eluted from the column filled up with the anion exchange resins 21 with 1 kmol/m 3 of hydrochloric acid solution to separate impurities such as molybdenum (Step S 106 ).
  • the obtained aqueous solution of iron chloride M was evaporated to dryness and oxidized to obtain iron oxide (Step S 107 ). And, the obtained iron oxide was heated to 1073 K (800° C.) in a hydrogen atmosphere to obtain iron (Step S 108 ).
  • the iron obtained in the Step S 108 was molten with plasma arc containing active hydrogen to remove impurities such as oxygen (Step S 109 ) to obtain high purity iron.
  • the invention is explained by the embodiments and examples. These embodiments and examples are not meant to limit the scope of the invention and variations within the concepts of the invention are apparent.
  • the copper may be absorbed on the anion exchange resins and be separated from the iron.
  • iron may be eluted with 0.1 kmol/m 3 to 6 kmol/m 3 of hydrochloric acid solution in order to separate the copper from the aqueous solution of iron chloride.
  • impurities other than copper may be removed by the methods as described in the above embodiments and examples, or by other conventional methods.
  • the copper may be separated as well as the impurities such as zinc from the aqueous solution of iron chloride after converting the trivalent iron ions to divalent iron ions as described above, or may be separated by other methods.
  • the contents of copper which causes influences such as a short circuit may be reduced to 50 mass ppb or less. Therefore, the high purity iron or the high purity iron targets according to the invention applied to semiconductor devices may not be responsible for short circuit of devices such as semiconductor devices and can provide the enhancement of properties of the semiconductor devices. Moreover, the high purity iron and the high purity iron targets can use for devices such as magnetic recording mediums and magnetic recording heads for the enhancement of properties. In addition, the high purity iron and the high purity iron targets used as materials of compound semiconductors such as iron silicide may not cause unwanted impurity level formed by small amounts of impurities responsible for property degradation and will provide good semiconductor properties.
  • the trivalent iron ions and the divalent copper ions are converted respectively to the divalent iron ions and the monovalent copper ions and the concentration of the hydrochloric acid is adjusted from 0.1 kmol/m 3 to 6 kmol/m 3 . Therefore, the copper may be absorbed on the anion exchange resins and be separated from the aqueous solution of iron chloride easily. In addition, the high purity iron and the high purity iron targets with low concentration of copper can be obtained easily and surely.
  • the trivalent iron ions are converted to the divalent iron ions and the concentration of the hydrochloric acid is adjusted from 0.1 kmol/m 3 to 6 kmol/m 3 . Therefore, the impurities such as zinc may be absorbed on the anion exchange resins and be separated from the aqueous solution of iron chloride easily. In addition, the high purity iron and the high purity iron targets can be obtained easily and surely.

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US20160068944A1 (en) * 2014-09-04 2016-03-10 Northwestern University Chemically pure zero-valent iron nanofilms from a low-purity iron source
US12046399B2 (en) * 2022-01-27 2024-07-23 Ford Global Technologies, Llc Reduction of cracks in additively manufactured Nd—Fe—B magnet

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JP4954479B2 (ja) * 2004-01-30 2012-06-13 ソニー株式会社 高純度電解鉄の製造方法および高純度電解コバルトの製造方法
JP4664719B2 (ja) * 2005-03-31 2011-04-06 鶴見曹達株式会社 塩化銅エッチング廃液の精製方法及び精製塩化銅溶液
JP5247986B2 (ja) * 2006-03-03 2013-07-24 株式会社田中化学研究所 高純度酸化鉄の製造方法
JP4723629B2 (ja) * 2008-11-13 2011-07-13 Ｊｘ日鉱日石金属株式会社 陰イオン交換樹脂を用いた銀の回収方法
KR101403281B1 (ko) * 2012-12-26 2014-06-03 재단법인 포항산업과학연구원 니켈 습식 제련 공정 부산물 회수 장치

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US20160068944A1 (en) * 2014-09-04 2016-03-10 Northwestern University Chemically pure zero-valent iron nanofilms from a low-purity iron source
US9738966B2 (en) * 2014-09-04 2017-08-22 Northwestern University Chemically pure zero-valent iron nanofilms from a low-purity iron source
US12046399B2 (en) * 2022-01-27 2024-07-23 Ford Global Technologies, Llc Reduction of cracks in additively manufactured Nd—Fe—B magnet

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KR20020025752A (ko) 2002-04-04
JP4323078B2 (ja) 2009-09-02
KR100854264B1 (ko) 2008-08-26
US20030206822A1 (en) 2003-11-06

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