US20160002749A1 - Method for manufacturing high purity manganese and high purity manganese - Google Patents

Method for manufacturing high purity manganese and high purity manganese Download PDF

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US20160002749A1
US20160002749A1 US14/770,843 US201414770843A US2016002749A1 US 20160002749 A1 US20160002749 A1 US 20160002749A1 US 201414770843 A US201414770843 A US 201414770843A US 2016002749 A1 US2016002749 A1 US 2016002749A1
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sublimation
high purity
ppm
ingot
distillation
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Kazuto Yagi
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JX Nippon Mining and Metals Corp
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    • 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
    • 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
    • C22B5/00—General methods of reducing to metals
    • C22B5/02—Dry methods smelting of sulfides or formation of mattes
    • C22B5/16—Dry methods smelting of sulfides or formation of mattes with volatilisation or condensation of the metal being produced
    • 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
    • C22B9/006—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals with use of an inert protective material including the use of an inert gas
    • 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
    • C22C—ALLOYS
    • C22C22/00—Alloys based on manganese
    • 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

Definitions

  • the present invention relates to a high purity manganese (Mn) manufactured from a commercially available electrolytic manganese (Mn) and a manufacturing method thereof.
  • a method for manufacturing a commercially available metal Mn is an electrolytic process in an ammonium sulfate electrolytic bath.
  • a commercially available electrolytic Mn obtained by this method contained are about 100 to 3000 ppm of sulfur (S) and several hundred ppm of carbon (C).
  • S sulfur
  • C carbon
  • CI chlorine
  • O oxygen
  • the sublimation purification method As a method for removing S, O from the above electrolytic Mn, the sublimation purification method is well known among conventional technologies. However, the sublimation purification method has disadvantages such as very expensive instrumentation and very poor yield. Further, even though the sublimation purification method can reduce S and O, a metal Mn obtained from the purification method will be subject to contamination due to the material of a heater, the material of a condenser and the like in a sublimation purification apparatus. For this reason, disadvantageously, it is not suitable as a raw material for electronic devices.
  • Patent Literature 1 describes a method for removing S in metal Mn in which, at a melting temperature of an Mn oxide compound such as MnO, Mn 3 O 4 and MnO 2 and/or metal Mn, a material to be converted into such an Mn oxide, for example Mn carbonate, is added, and metal Mn to which an Mn compound has been added is melted under an inert atmosphere, and maintained in a molten state preferably for 30 to 60 minutes to give a sulfur content of 0.002%.
  • an Mn oxide compound such as MnO, Mn 3 O 4 and MnO 2 and/or metal Mn
  • Literature 1 does not contain any description about the contents of oxygen (O), nitrogen (N), carbon (C) and chlorine (CI), and does not provide a solution for a problem that is caused when these materials are contained.
  • Patent Literature 2 describes a method for electrowinning metal Mn, and a method for electrowinning metal Mn characterized in that used is an electrolytic solution prepared by dissolving an excess amount of a high purity metal Mn in hydrochloric acid, filtering out undissolved materials to obtain a solution, neutralizing the solution by the addition of an oxidizing agent, filtering out the resulting precipitates, and then adding a buffering agent.
  • electrowinning metal Mn with the use of an electrolytic solution prepared by further adding metal Mn to a hydrochloric acid solution of a metal Mn, filtering out undissolved materials to obtain a solution, adding hydrogen peroxide and aqueous ammonia to the solution, filtering out precipitates formed under weakly acidic or neutral pH, and then adding a buffering agent.
  • Literature 2 describes that S in a high purity Mn is reduced to 1 ppm, it does not have any description about the contents of oxygen (O), nitrogen (N), carbon (C) and chlorine (Cl), and does not provide a solution for a problem that is caused when these materials are contained.
  • Patent Literature 3 describes a method for manufacturing a high purity Mn, and a method in which an ion-exchange purification method using a chelating resin is applied to an aqueous Mn chloride, and then the resulting purified aqueous Mn chloride is highly purified by the electrowinning method. It is described that in a dry process, a high purity Mn can be obtained from solid phase Mn by the vacuum sublimation purification method (Mn vapor obtained by sublimation of solid phase Mn is selectively condensed and deposited as a purified material at a cooling unit due to the difference in vapor pressures).
  • Literature 3 describes that the total concentration of sulfur (S), oxygen (O), nitrogen (N) and carbon (C) is 10 ppm or less.
  • Literature 3 does not contain any description about the content of chlorine (Cl) which has a deleterious effect on the manufacture of semiconductor components.
  • Mn chloride is used as a raw material, and therefore, disadvantageously, chlorine may be contained at a high concentration.
  • Patent Literature 4 describes a method for manufacturing a low-oxygen Mn material in which an Mn material with oxygen reduced to 100 ppm or less can be obtained by performing induction skull melting to an Mn raw material under an inert gas atmosphere, and the Mn raw material is preferably subjected to an acid wash before induction skull melting in view of further reducing oxygen.
  • Literature 4 has a description about the reduction of oxygen (O), sulfur (S) and nitrogen (N) in a high purity Mn, it does not have any description about the content of the other impurities, and does not provide a solution for a problem caused when these materials are contained.
  • Patent Literature 5 describes an Mn alloy material for magnetic materials, an Mn alloy sputtering target, and a magnetic thin film. Also described is that the content of oxygen (O) is 500 ppm or less, the content of sulfur (S) is 100 ppm or less, and further, the total content of impurities (elements other than Mn and alloy components) is preferably 1000 ppm or less. Further, the Literature describes a method for removing oxygen (O) and sulfur (S) by adding, as deoxidizing/desulfurizing agents, Ca, Mg, La and the like to a commercially available electrolytic Mn and then performing high frequency melting. It also describes that vacuum distillation is performed after preliminary melting for being highly purified.
  • Example 3 a deoxidizing/desulfurizing agent is added, and then high frequency melting is performed to give an oxygen content of 50 ppm and a sulfur content of 10 ppm (Table 3).
  • Example 7 vacuum distillation is performed after preliminary melting to give an oxygen content of 30 ppm and a sulfur content of 10 ppm (Table 7).
  • about 10 to 20 ppm of Si and about 10 to 30 ppm of Pb are contained.
  • Example 3 of the following Patent Literature 5 high frequency melting is performed after adding a deoxidizing/desulfurizing agent. Therefore, disadvantageously, a deoxidizing/desulfurizing agent may contaminate Mn to reduce the purity.
  • vacuum distillation is performed after preliminary melting. Therefore, disadvantageously, a manufacturing cost is high because 99% or more of dissolved Mn is subject to volatilization.
  • Patent Literature 6 describes a method for manufacturing a high purity Mn material and a high purity Mn material for forming a thin film.
  • preliminary melting of crude Mn is performed at 1250 to 1500° C.
  • vacuum distillation is performed at 1100 to 1500° C. to obtain a high purity Mn material.
  • the degree of vacuum when performing vacuum distillation is preferably 5 ⁇ 10 ⁇ 5 to 10 Torr.
  • the total impurity content in a high purity Mn obtained as described above is 100 ppm or less: Oxygen (O): 200 ppm or less, Nitrogen (N): 50 ppm or less, Sulfur (S): 50 ppm or less and Carbon (C): 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.
  • the oxygen content is 30 ppm, and other elements are contained less than 10 ppm in Example 2 (Table 2).
  • the impurity level has not reached the intended level.
  • Patent Literature 7 describes a sputtering target comprising a high purity Mn alloy.
  • Patent Literature 8 describes a method for recovering Mn using sulfuric acid.
  • Patent Literature 9 describes a method for manufacturing metal Mn in which Mn oxide is subjected to heat reduction.
  • none of the above describes desulfurization in particular.
  • the present inventors have proposed a method for manufacturing a high purity Mn, comprising leaching an Mn raw material in acid, filtering out residues and using the filtrate for the cathode side in electrolysis; the above method for manufacturing a high purity Mn, further comprising degassing the above electrolytic Mn to reduce the CI content in the above electrolytic Mn to 100 ppm or less; and the method for manufacturing a high purity Mn, further comprising degassing the above electrolytic Mn material, and performing melting under an inert atmosphere to manufacture Mn where Cl ⁇ 10 ppm, C ⁇ 50 ppm, S ⁇ 50 ppm, and O ⁇ 30 ppm (see Patent Literature 10).
  • An object of the present invention is to provide a manufacturing method capable of achieving a higher purity and reducing cost. Another object is to provide a high purity Mn.
  • An object of the present invention is to provide a high purity Mn manufactured from a commercially available electrolytic Mn and a manufacturing method thereof.
  • the present invention aims to provide a high purity Mn that has a significantly lower impurity content and is manufactured at a lower cost as compared with the conventional technology.
  • the present invention solves the above problems, and provides the following invention.
  • a method for manufacturing a high purity Mn comprising: placing an Mn raw material in a magnesia crucible to perform melting with the use of a vacuum induction melting furnace (VIM furnace) at a melting temperature of 1240 to 1400° C.
  • VIM furnace vacuum induction melting furnace
  • a high purity Mn according to any one of 1) to 4), comprising, when the deposited amount of sublimated/distilled Mn reaches 70% of the weight of the metal Mn ingot charged into the alumina crucible during the sublimation/distillation step, stopping the sublimation/distillation step.
  • the gas component elements in the present invention mean hydrogen (H), oxygen (O), nitrogen (N), and carbon (C). The same hereinafter.
  • ppm means “wtppm”. Except for nitrogen (N) and oxygen (O) which are gas component elements, analytical values for the concentration of each element were analyzed with the GDMS (Glow Discharge Mass Spectrometry) method. Moreover, gas component elements were analyzed using an oxygen/nitrogen analyzer from LECO Corporation.
  • the present invention provides the following effects.
  • a high purity Mn which has a purity of 4N5 (99.995%) or more except for gas components, and in which the total amount of impurity elements B, Mg, Al, Si, S, Ca, Cr, Fe and Ni is 50 ppm or less, can be obtained. Further a high purity Mn, which has a purity of 5N (99.999%) or more except for gas components, and in which the total amount of impurity elements B, Mg, Al, Si, S, Ca, Cr, Fe and Ni is 10 ppm or less, can be obtained. (2) Further each of O and N as gas components can be reduced to less than 10 ppm. (3) Without the need for special equipment, a common furnace can be used for manufacturing a high purity Mn at a lower cost and higher yield as compared with the conventional distillation method.
  • FIG. 1 This shows a schematic diagram of a sequence of process steps from a step of subjecting the Mn raw material to primary VIM (vacuum induction melting), a secondary VIM step, and a sublimation and distillation purification step through to the manufacture of highly purified Mn.
  • primary VIM vacuum induction melting
  • secondary VIM sublimation and distillation purification step
  • an Mn raw material is placed in a magnesia crucible, and subjected to melting with the use of a vacuum induction melting furnace (VIM furnace) at a melting temperature of 1240 to 1400° C. under an inert atmosphere of 500 Torr or less (primary VIM step).
  • VIP furnace vacuum induction melting furnace
  • Mn does not melt, and the VIM treatment cannot be performed. If the temperature is more than 1400° C., suspended materials of oxides and/or sulfides are re-melted into Mn due to the high temperature. Therefore, the concentrations of magnesium (Mg), calcium (Ca), oxygen (O) and sulfur (S) after the primary VIM step will be in an order of hundreds of ppm to thousands of ppm, and the intended purity in the present invention ultimately cannot be achieved. Results are shown in Table 2.
  • this Mn ingot is placed in a magnesia crucible to perform melting with the use of a vacuum induction melting furnace (VIM furnace) at a melting temperature, which is adjusted to 1200 to 1450° C. and maintained for 10 to 60 minutes, under an inert atmosphere of 200 Torr or less (secondary VIM step). Then, the resultant is cast in an iron mold to manufacture an ingot. After cooling the ingot, slags adhered to the ingot are removed.
  • VIM furnace vacuum induction melting furnace
  • the primary VIM step since Ca as a deoxidizing/desulfurizing agent is added to molten Mn during melting, a small amount of Ca is contained in an Mn ingot after the primary melting, and the melting point of Mn decreases. Therefore, even in a case where a temperature of the secondary VIM is in a temperature range lower than that of the primary VIM, melting can be performed.
  • the deoxidizing/desulfurizing agent (Ca) added during the primary VIM step can be removed.
  • a temperature of the secondary VIM is more than 1450° C., volatilization loss of Mn significantly increases, resulting in a decreased yield and increased cost; therefore, it is not preferable.
  • this metal Mn ingot is placed in an alumina crucible, the pressure is reduced to 0.01 to 1 Torr with a vacuum pump, and then heating is performed.
  • a sublimation/distillation reaction is developed at a sublimation/distillation temperature of 1100 to 1250° C. to manufacture a high purity Mn.
  • Mn volatilized by the sublimation/distillation reaction is guided to a cooling cylinder where deposited Mn is recovered.
  • the sublimation/distillation step is stopped when the amount of Mn recovered in the sublimation/distillation reaction reaches 70% of the weight of the Mn material charged in the alumina crucible.
  • This stop operation can prevent impurity elements which remain in the crucible from sublimating to contaminate Mn deposited in the cooling cylinder to reduce the purity.
  • the outlines of this step are shown in FIG. 1 .
  • Mn obtained by this manufacturing method a high purity Mn having a purity of 4N5 (99.995%) or more except for gas components in which the sum (the total amount) of impurity elements, B, Mg, Al, Si, 5 , Ca, Cr, Fe and Ni is 50 ppm or less can be obtained.
  • a high purity Mn having a purity of 5N (99.999%) or more in which the sum (the total amount) of impurity elements, B, Mg, Al, Si, S, Ca, Cr, Fe and Ni is 10 ppm or less can be obtained.
  • purification can be performed at a sublimation/distillation temperature of 1200 to 1250° C.
  • each of O and N as gas components can be reduced to less than 10 ppm.
  • a high purity Mn can be obtained by placing a metal Mn ingot in a cylindrical alumina crucible for performing the sublimation and distillation; vertically aligning a similarly-shaped alumina cylinder on top of the above cylindrical crucible; and developing a sublimation and distillation reaction to deposit Mn inside the upper alumina cylinder.
  • the structure is simple as cylindrical alumina crucibles (cylinders) are piled, and equipment with such a structure contributes to the reduction in a manufacturing cost.
  • the duration of sublimation/distillation purification is about 8 to 75 hours.
  • the sublimation/distillation rate is preferably 20 to 184 g/h, more preferably 103 to 184 g/h.
  • the sublimation/distillation reaction step was stopped when the amount of Mn recovered by deposition reached 70% (recovery rate) of the weight of the Mn raw material charged in the alumina crucible.
  • the impurity concentrations in the raw material Mn increase, and impurity elements are sublimated more significantly at the final stage of the step. Therefore, contamination of impurities into the distilled Mn can be prevented by stopping the step when Mn recovered by deposition reaches 70 wt % of the weight of the raw material Mn.
  • a commercially available flake-like electrolytic Mn (purity 2N: 99%) was used. Impurities in the raw material Mn were 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 to 2500 ppm, and N: 10 to 20 ppm.
  • the above Mn raw material was placed in a magnesia crucible, and melting was performed using a vacuum induction melting furnace (VIM furnace) at a melting temperature of 1300° C. under an inert atmosphere of 200 Torr or less. Then, Ca in 1 wt % of the weight of Mn was gradually added to this molten Mn to perform deoxidation and desulfurization. After the completion of the deoxidation and desulfurization, the resultant was cast in an iron mold to manufacture an ingot. After cooling the ingot, slags adhered to the ingot were removed.
  • VIP furnace vacuum induction melting furnace
  • Impurities in the ingot after this primary melting were B: 12 ppm, Mg: 130 ppm, Al: 1.2 ppm, Si: 20 ppm, S: 3.4 ppm, Ca: 520 ppm, Cr: 0.25 ppm, Fe: 2.2 ppm, Ni: 1.4 ppm, O: 10 ppm, and N: 10 ppm. Results are shown in Table 1.
  • the Mn ingot obtained from the primary VIM was placed in a magnesia crucible, and a secondary VIM was performed using a vacuum induction melting furnace (VIM furnace) at a melting temperature, which was adjusted to 1400° C. and maintained for 30 minutes, under an inert atmosphere of 100 Torr or less. Then, the resultant was cast in an iron mold to manufacture an ingot. After cooling the ingot, slags adhered to the ingot were removed.
  • VIM furnace vacuum induction melting furnace
  • Impurities in the ingot after this secondary melting were B: 10 ppm, Mg: 13 ppm, Al: 1.9 ppm, Si: 20 ppm, S: 0.58 ppm, Ca: 25 ppm, Cr: 0.28 ppm, Fe: 2.4 ppm, Ni: 1.2 ppm, O: 10 ppm, and N: 10 ppm. Results are also shown in Table 1.
  • the metal Mn ingot obtained through the above primary VIM step and the secondary VIM step was placed in a cylindrical alumina crucible, and a similarly-shaped alumina cylinder was vertically aligned on top of this cylindrical crucible to develop a sublimation and distillation reaction.
  • Mn in the cylindrical alumina crucible was heated to 1050 to 1250° C., and the sublimation rate was 3 to 184 g/h. In this case, the duration of sublimation purification was about 8 to 75 hours.
  • the impurity removing effect of sublimation/distillation purification is significantly affected by the heating temperature and the sublimation/distilling rate. Therefore, it is performed in varying temperatures within a range of 1050 to 1250° C. and sublimation/distilling rates within a range of 3 to 184 g/h, as described above. Specific examples (Examples and Comparative Examples) are shown below.
  • the sublimation/distillation step was stopped when the amount of Mn recovered in the sublimation/distillation reaction reached 70% (recovery rate) of the weight of the Mn raw material charged in the alumina crucible to prevent the distilled Mn from being contaminated by impurities.
  • the relationship between the heating temperature and the sublimation/distillation rate is preliminarily investigated, and the amount of Mn to be deposited in a sublimation/distillation rate at each heating temperature is calculated to determine the time to stop the step.
  • impurities in the metal Mn after this sublimation purification were B: 0.2 ppm, Mg: 20 ppm, Al: 0.15 ppm, Si: 0.05 ppm, S: 0.03 ppm, Ca: 30 ppm, Cr: 0.05 ppm, Fe ⁇ 0.1 ppm, Ni: 0.01 ppm, O ⁇ 10 ppm, and N ⁇ 10 ppm. Results are shown in Table 1.
  • Sublimation/distillation purification was performed at a heating temperature of 1100° C. and a sublimation rate of 23 (g/h).
  • Impurities in the metal Mn after this sublimation purification were B: 0.61 ppm, Mg: 17 ppm, Al: 0.25 ppm, Si: 0.28 ppm, S: 0.07 ppm, Ca: 7.3 ppm, Cr: 0.05 ppm, Fe ⁇ 0.1 ppm, Ni: 0.03 ppm, O ⁇ 10 ppm, and N ⁇ 10 ppm. Results are shown in Table 1 as well.
  • Sublimation/distillation purification was performed at a heating temperature of 1200° C. and a sublimation rate of 103 (g/h).
  • Impurities in the metal Mn after this sublimation purification were B: 0.46 ppm, Mg: 0.17 ppm, Al: 1.4 ppm, Si: 1.2 ppm, S: 0.02 ppm, Ca: 2.1 ppm, Cr: 0.69 ppm, Fe: 0.21 ppm, Ni: 0.08 ppm, O ⁇ 10 ppm, and N ⁇ 10 ppm. Results are also shown in Table 1 as well.
  • Sublimation/distillation purification was performed at a heating temperature of 1250° C. and a sublimation rate of 184 (g/h).
  • Impurities in the metal Mn after this sublimation purification were B: 1.1 ppm, Mg ⁇ 0.01 ppm, Al: 0.85 ppm, Si: 3.6 ppm, S: 0.04 ppm, Ca: 1.9 ppm, Cr: 1.4 ppm, Fe: 0.77 ppm, Ni: 0.18 ppm, O ⁇ 10 ppm, and N ⁇ 10 ppm. Results are shown in Table 1 as well.
  • Mn having ultra-high purity can be obtained by a relatively simple manufacturing process at a reduced manufacturing cost. Therefore, it is useful as: a metal Mn used for wiring materials, electronic component materials such as magnetic materials (magnetic recording heads), and semiconductor component materials; and a sputtering target material for forming a thin film thereof, in particular an Mn-containing thin film. Since the present invention can be manufactured with a common furnace without the need for special equipment, and a high purity Mn can be obtained at a lower cost and higher yield as compared with the conventional distillation method, it can be said that it has high value regarding industrial use.

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US11242595B1 (en) 2021-04-03 2022-02-08 King Faisal University Method of making metal nanostructures using low temperature deposition

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