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WO2015060026A1 - Procédé de production de manganèse de pureté élevée et manganèse de pureté élevée - Google Patents

Procédé de production de manganèse de pureté élevée et manganèse de pureté élevée Download PDF

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Publication number
WO2015060026A1
WO2015060026A1 PCT/JP2014/073615 JP2014073615W WO2015060026A1 WO 2015060026 A1 WO2015060026 A1 WO 2015060026A1 JP 2014073615 W JP2014073615 W JP 2014073615W WO 2015060026 A1 WO2015060026 A1 WO 2015060026A1
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WO
WIPO (PCT)
Prior art keywords
purity
ppm
less
melting
high purity
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
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PCT/JP2014/073615
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English (en)
Japanese (ja)
Inventor
和人 八木
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
JX Nippon Mining and Metals Corp
Original Assignee
JX Nippon Mining and Metals Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by JX Nippon Mining and Metals Corp filed Critical JX Nippon Mining and Metals Corp
Priority to JP2015518497A priority Critical patent/JP6050485B2/ja
Priority to KR1020167029451A priority patent/KR20160125537A/ko
Priority to KR1020157028532A priority patent/KR101678334B1/ko
Priority to US14/777,064 priority patent/US20160032427A1/en
Publication of WO2015060026A1 publication Critical patent/WO2015060026A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • C22B47/00—Obtaining manganese
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D7/00—Casting ingots, e.g. from ferrous metals
    • B22D7/005—Casting ingots, e.g. from ferrous metals from non-ferrous metals
    • 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
    • C22B47/00—Obtaining manganese
    • C22B47/0018—Treating ocean floor nodules
    • C22B47/009—Treating ocean floor nodules refining, e.g. separation of metals obtained by the above methods
    • 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
    • C22B9/003—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals by induction
    • 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
    • C22B9/04—Refining by applying a vacuum
    • 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
    • C22B9/10—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals with refining or fluxing agents; Use of materials therefor, e.g. slagging or scorifying agents
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C22/00—Alloys based on manganese

Definitions

  • the present invention relates to high-purity manganese (Mn) from commercially available electrolytic manganese (Mn) and a method for producing the same.
  • a commercially available method for producing metal Mn is an electrolytic method from an ammonium sulfate electrolytic bath.
  • sulfur (S) is about 100 to 3000 ppm
  • carbon (C) is also several hundred ppm.
  • Chlorine (Cl) is also several hundred ppm
  • oxygen (O) is contained in the order of several thousand ppm because it is an electrodeposit from the aqueous solution.
  • a sublimation purification method As a method for removing S and O from the electrolytic Mn, a sublimation purification method is well known in the prior art.
  • the sublimation purification method has a problem that the apparatus is very expensive and the yield is very bad.
  • S and O can be reduced by the sublimation purification method, it is contaminated due to the heater material, condenser material, etc. of the sublimation purification device, so metal Mn by the purification method is used as a raw material for electronic devices. There was a problem that it was not suitable.
  • Patent Document 1 a method for removing S in metal Mn is described in Patent Document 1 below, and Mn oxidation is performed at a melting temperature of Mn acid compounds such as MnO, Mn 3 O 4 , MnO 2 and / or metal Mn.
  • Mn acid compounds such as MnO, Mn 3 O 4 , MnO 2 and / or metal Mn.
  • Mn carbonate or the like is added, and the metal Mn to which the Mn compound is added is melted in an inert atmosphere and kept in a molten state, preferably for 30 to 60 minutes, and the S content: 0.002% It is described that.
  • this document 1 does not describe the contents of oxygen (O), nitrogen (N), carbon (C), and chlorine (Cl) at all, and has not yet solved the problems caused by the contents thereof. .
  • Patent Document 2 a method for electrolytically collecting metal Mn and high-purity metal Mn are dissolved in hydrochloric acid, and an undissolved material is filtered.
  • a method for electrolytic collection of metal Mn characterized by using an electrolyte prepared by filtering a product and adding a buffer, preferably adding metal Mn to a hydrochloric acid solution of metal Mn, Using electrolyte prepared by adding hydrogen peroxide and aqueous ammonia to the solution obtained by filtering undissolved material, filtering the precipitate formed under weakly acidic or neutral liquidity, and adding a buffer.
  • a method of performing electrowinning of metal Mn is described.
  • Patent Document 3 describes a method for producing high-purity Mn.
  • An ion-exchange purification method using a chelate resin is applied to an aqueous Mn chloride solution, and then the purified aqueous Mn chloride solution is purified by electrowinning. How to do is described.
  • the dry method describes that high-purity Mn is obtained from solid-phase Mn by vacuum sublimation purification method (Mn vapor obtained by sublimation of solid-phase Mn is selectively condensed and vapor-deposited in the cooling section by vapor pressure difference). Has been.
  • the document 3 describes that the total concentration of sulfur (S), oxygen (O), nitrogen (N), and carbon (C) is 10 ppm or less. However, this document 3 does not describe the content of chlorine (Cl) that is harmful to the manufacture of semiconductor components. Since Mn chloride is used as a raw material, there is a possibility that chlorine may be contained in a high concentration, which is problematic.
  • Patent Document 4 describes a method for producing a low-oxygen Mn material, and obtains a Mn material in which the oxygen content is reduced to 100 ppm or less by inductively skull-dissolving the Mn raw material in an inert gas atmosphere. There is a description that it is preferable to perform acid cleaning before induction skull dissolution of the Mn raw material because oxygen can be further reduced. However, in this document 4, there is a description regarding the reduction of oxygen (O), sulfur (S), and nitrogen (N) in high-purity Mn, but there is no description regarding the content of other impurities. The problem of inclusion has not been solved.
  • Patent Document 5 describes a Mn alloy material for magnetic materials, a Mn alloy sputtering target, and a magnetic thin film, and has an oxygen content of 500 ppm or less and an S content of 100 ppm or less, preferably further impurities (Mn and alloy components). It is described that the total content of elements other than the above is 1000 ppm or less. Furthermore, the same literature describes a method for removing oxygen (O) and sulfur (S) by adding Ca, Mg, La, etc. as a deoxidizing / desulfurizing agent to commercially available electrolytic Mn, and performing high-frequency dissolution, It describes that it is purified by vacuum distillation after preliminary dissolution.
  • O oxygen
  • S sulfur
  • Example 3 In the above Mn raw material, in Example 3, a deoxidizing / desulfurizing agent was added and high-frequency dissolution was performed to obtain an oxygen content of 50 ppm and a sulfur content of 10 ppm (Table 3 of Patent Document 5). There is a description that the oxygen content is 30 ppm and the sulfur content is 10 ppm (Table 7 of Patent Document 5) by distillation. In these examples, Si is contained in an amount of about 10 to 20 ppm and Pb is contained in an amount of about 10 to 30 ppm.
  • Example 3 of Patent Document 5 below since the deoxidation / desulfurization agent is added and dissolved at high frequency, there is a problem that the deoxidation / desulfurization agent is mixed in Mn and lowers the purity. Has been subjected to vacuum distillation after pre-dissolution and volatilizes 99% or more of the dissolved Mn, which has a problem of high production cost.
  • Patent Document 6 describes a method for producing a high-purity Mn material and a high-purity Mn material for forming a thin film.
  • a high-purity Mn material is obtained by pre-dissolving crude Mn at 1250-1500 ° C. and then vacuum distillation at 1100-1500 ° C.
  • the degree of vacuum during vacuum distillation 5 ⁇ 10 - and 5 ⁇ 10 Torr.
  • the high-purity Mn thus obtained has a total impurity content of 100 ppm or less, oxygen (O): 200 ppm or less, nitrogen (N): 50 ppm or less, sulfur (S): 50 ppm or less, carbon (C): 100 ppm or less.
  • Example 2 (Table 2) describes an example in which oxygen is 30 ppm and other elements are less than 10 ppm. However, also in this case, the impurity level does not reach the target level.
  • Patent Document 7 describes a sputtering target made of a high-purity Mn alloy
  • Patent Document 8 describes a method of recovering Mn using sulfuric acid
  • Patent Document 9 produces metal Mn by heat reduction of Mn oxide.
  • desulfurization there is no description regarding desulfurization.
  • the present inventors leached the Mn raw material with an acid, filtered the residue with a filter, and then used the filtered solution on the cathode side in electrolysis, and also removed the electrolytic Mn.
  • a high-purity Mn production method for producing Mn with ⁇ 50 ppm, S ⁇ 50 ppm, and O ⁇ 30 ppm was proposed (see Patent Document 10). This method is effective for increasing the purity of Mn.
  • the present invention is aimed at a manufacturing method and high-purity Mn that can achieve higher purity and can reduce costs.
  • An object of the present invention is to provide a high-purity Mn from a commercially available electrolytic Mn and a method for producing the same, and in particular, to produce a high-purity Mn with a lower amount of impurities and at a lower cost than the prior art. Let it be an issue.
  • a method for producing high-purity Mn in which a Mn raw material is placed in a magnetic crucible and melted at a melting temperature of 1240 to 1400 ° C. in an inert atmosphere of 500 Torr or less using a vacuum induction melting furnace (VIM furnace).
  • VIM furnace vacuum induction melting furnace
  • Calcium (Ca) is added in the range of 0.5 to 2.0% of the Mn weight to perform deoxidation and desulfurization, and after completion of the deoxidation and desulfurization, an ingot is produced by casting into an iron mold.
  • a Mn ingot is loaded into a skull melting furnace, heated by reducing the pressure to 10 ⁇ 5 Torr or less with a vacuum pump, and after maintaining the molten state for 10 to 60 minutes, the melting reaction is terminated to obtain high purity Mn.
  • a method for producing high-purity Mn is described in detail below.
  • the total amount of impurity elements B, Mg, Al, Si, S, Ca, Cr, Fe, and Ni is 50 ppm or less, and has a purity of 4N5 (99.995%) or more excluding gas component elements.
  • High-purity Mn characterized by
  • the total amount of impurity elements B, Mg, Al, Si, S, Ca, Cr, Fe, and Ni is 50 ppm or less, and has a purity of 4N5 (99.995%) or more excluding gas component elements.
  • the unit “ppm” used in this specification means “wtppm”. Except for nitrogen (N) and oxygen (O) which are gas component elements, analysis values of each element concentration are GDMS (Glow Discharge). The analysis was performed by Mass Spectrometry, and the gas component elements (O, N) were analyzed using an oxygen-nitrogen analyzer manufactured by LECO.
  • the gas component element in the present invention means hydrogen (H), oxygen (O), nitrogen (N), and carbon (C). The following also means the same.
  • the present invention has the following effects. (1) High-purity Mn having a total amount of impurity elements B, Mg, Al, Si, S, Ca, Cr, Fe, and Ni of 50 ppm or less and a purity of 4N5 (99.995%) or more; It is possible to obtain high-purity Mn in which O and N as gas components can each be less than 10 ppm.
  • the method for producing high-purity Mn according to the present invention can use commercially available (2N level) flaky electrolytic Mn as a raw material, but since it does not affect the purity of the raw material, the type of the raw material is not particularly limited.
  • a Mn raw material is put in a magnesia crucible and melted at a melting temperature of 1240 to 1400 ° C. in an inert atmosphere of 500 Torr or less using a vacuum induction melting furnace (VIM furnace). If it is less than 1240 ° C., VIM treatment cannot be performed because Mn does not melt.
  • VIM furnace vacuum induction melting furnace
  • Mn obtained by this production method has a total amount of impurity elements B, Mg, Al, Si, S, Ca, Cr, Fe, and Ni of 50 ppm or less, and 4N5 (99.995% excluding gas components) ) High purity Mn having the above purity.
  • the total amount of impurity elements B, Mg, Al, Si, S, Ca, Cr, Fe, and Ni is 50 ppm or less, and O and N that are gas components can each be less than 10 ppm.
  • O and N in electronic devices using Mn forms oxides or nitrides, which not only deteriorates the properties of Mn itself, but also oxidizes in composites or alloyed materials with Mn.
  • the influence of the formation of nitrides or nitrides (deterioration of characteristics) or the influence of diffusion of O or N (deterioration of characteristics) between adjacent materials may occur.
  • the presence of Mn, which can be reduced, is extremely effective. A summary of these steps is shown in FIG.
  • a normal skull dissolution apparatus For skull dissolution, a normal skull dissolution apparatus can be used. In general, the skull furnace is cooled, and the raw material charged in the furnace is melted by induction heating, so that there is no contamination from the furnace. In the purification of Mn, VIM dissolution removes S and O in advance with calcium (Ca), and then the skull furnace is used to remove the extremely increased Mg and Ca, and finally increase the purity of Mn. It can be said that the idea of aiming did not exist in the prior art.
  • Example 1 Commercially available flaky electrolytic Mn (purity 2N: 99%) was used as a starting material.
  • the impurities of the raw material Mn are B: 15 ppm, Mg: 90 ppm, Al: 4.5 ppm, Si: 39 ppm, S: 280 ppm, Ca: 5.9 ppm, Cr: 2.9 ppm, Fe: 11 ppm, Ni: 10 ppm, O: 720-2500 ppm, N: 10-20 ppm.
  • VIM dissolution process The Mn raw material was placed in a magnetic crucible and melted at a melting temperature of 1300 ° C. in an inert atmosphere of 200 Torr or less using a vacuum induction melting furnace (VIM furnace). And 1 weight% of calcium (Ca) of Mn weight was gradually added to this Mn molten metal, and deoxidation and desulfurization were performed. After completion of deoxidation and desulfurization, an ingot was manufactured by casting a molten Mn into an iron mold. After the ingot was cooled, the slag adhering to the ingot was removed.
  • Impurities in the ingot after dissolution were B: 14 ppm, Mg: 160 ppm, Al: 1.2 ppm, Si: 16 ppm, S: 16 ppm, Ca: 520 ppm, Cr: 2.5 ppm, Fe: 3.6 ppm, Ni: 1 .3 ppm, O: less than 10 ppm, and N: less than 10 ppm.
  • the results are shown in Table 1.
  • the Mn ingot obtained by the above VIM melting is filled in a water-cooled crucible, the crucible is placed in a skull melting furnace, is made 10 ⁇ 5 Torr or less by a vacuum pump, heated by induction heating, After confirming the melting of a certain Mn ingot, the melting was terminated for 30 minutes, and solidified Mn was obtained.
  • Impurities of this Mn ingot were B: 8.1 ppm, Mg: 1.9 ppm, Al: 1.7 ppm, Si: 16 ppm, S: 2.7 ppm, Ca: 9.4 ppm, Cr: 1.1 ppm, Fe: 3 0.6 ppm, Ni: 1.1 ppm, O: less than 10 ppm, and N: less than 10 ppm.
  • the electrolytic Mn raw material with a purity of 2N could be highly purified to 4N5 except for gas component elements.
  • Mn with extremely high purity can be obtained, the manufacturing process is relatively simple, and the manufacturing cost can be reduced. Therefore, electronic component materials such as wiring materials and magnetic materials (magnetic heads), semiconductor components, etc. It is useful as a sputtering target material for producing a metal Mn used for the material, the same thin film, particularly a Mn-containing thin film. Since the present invention can be produced in a general-purpose furnace without requiring a special apparatus and can obtain high-purity Mn at a low cost and in a high yield as compared with the conventional distillation method, It can be said that the utility value of is high.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Oceanography (AREA)
  • Ocean & Marine Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Mold Materials And Core Materials (AREA)

Abstract

La présente invention concerne un procédé de production de Mn de pureté élevée, le procédé étant caractérisé en ce que : un produit de départ de Mn est placé dans un creuset en magnésie et est fondu à une température de fusion située dans la plage allant de 1 240 à 1 400 °C à l'aide d'un four de fusion par induction sous vide (four VIM) sous une atmosphère inerte de pression inférieure ou égale à 500 Torr ; du calcium est ajouté dans une plage allant de 0,5 à 2,0 % du poids de Mn pour réaliser une désoxygénation et une désulfuration ; après achèvement de la désoxygénation et de la désulfuration, un lingot est fabriqué par coulée dans un moule en fer ; puis ledit lingot de Mn est chargé dans un four de fusion à fond de moule refroidi, la pression est réduite à une pression inférieure ou égale à 10-5 Torr au moyen d'une pompe à vide, et le chauffage est mis en route ; et après avoir maintenu l'état de fusion pendant 10 à 60 minutes, la réaction de fusion est terminée pour obtenir du Mn de pureté élevée. La présente invention concerne un procédé de production de Mn métal de pureté élevée à partir de Mn électrolytique disponible dans le commerce. En particulier, la présente invention aborde le problème de l'obtention de Mn métal de pureté élevée contenant de faibles quantités d'impuretés telles que B, Mg, Al et Si.
PCT/JP2014/073615 2013-10-25 2014-09-08 Procédé de production de manganèse de pureté élevée et manganèse de pureté élevée Ceased WO2015060026A1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
JP2015518497A JP6050485B2 (ja) 2013-10-25 2014-09-08 高純度マンガンの製造方法及び高純度マンガン
KR1020167029451A KR20160125537A (ko) 2013-10-25 2014-09-08 고순도 망간
KR1020157028532A KR101678334B1 (ko) 2013-10-25 2014-09-08 고순도 망간의 제조 방법
US14/777,064 US20160032427A1 (en) 2013-10-25 2014-09-08 Method for manufacturing high purity manganese and high purity manganese

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2013222139 2013-10-25
JP2013-222139 2013-10-25

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WO2015060026A1 true WO2015060026A1 (fr) 2015-04-30

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US (1) US20160032427A1 (fr)
JP (1) JP6050485B2 (fr)
KR (2) KR101678334B1 (fr)
TW (1) TW201527541A (fr)
WO (1) WO2015060026A1 (fr)

Cited By (2)

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Publication number Priority date Publication date Assignee Title
JP2021088744A (ja) * 2019-12-04 2021-06-10 株式会社 大阪アサヒメタル工場 高純度マンガンの製造方法および高純度マンガン
CN115491533A (zh) * 2022-09-29 2022-12-20 贵州松桃金瑞锰业有限责任公司 一种锰合金的制备方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113088828B (zh) * 2021-03-25 2022-04-19 江苏省沙钢钢铁研究院有限公司 一种高Mn高Al钢及其真空熔炼工艺
CN116219182A (zh) * 2023-01-04 2023-06-06 宁波创润新材料有限公司 一种锰添加剂及其制备方法

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WO2013111609A1 (fr) * 2012-01-23 2013-08-01 Jx日鉱日石金属株式会社 Cible de pulvérisation d'alliage cuivre-manganèse de grande pureté

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WO2013111609A1 (fr) * 2012-01-23 2013-08-01 Jx日鉱日石金属株式会社 Cible de pulvérisation d'alliage cuivre-manganèse de grande pureté

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Publication number Priority date Publication date Assignee Title
JP2021088744A (ja) * 2019-12-04 2021-06-10 株式会社 大阪アサヒメタル工場 高純度マンガンの製造方法および高純度マンガン
JP7298893B2 (ja) 2019-12-04 2023-06-27 株式会社 大阪アサヒメタル工場 高純度マンガンの製造方法および高純度マンガン
JP2023107868A (ja) * 2019-12-04 2023-08-03 株式会社 大阪アサヒメタル工場 高純度マンガンの製造方法および高純度マンガン
JP7594808B2 (ja) 2019-12-04 2024-12-05 株式会社 大阪アサヒメタル工場 高純度マンガンの製造方法および高純度マンガン
CN115491533A (zh) * 2022-09-29 2022-12-20 贵州松桃金瑞锰业有限责任公司 一种锰合金的制备方法

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JPWO2015060026A1 (ja) 2017-03-09
US20160032427A1 (en) 2016-02-04
JP6050485B2 (ja) 2016-12-21
KR20150125721A (ko) 2015-11-09
KR101678334B1 (ko) 2016-11-21
KR20160125537A (ko) 2016-10-31
TW201527541A (zh) 2015-07-16

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