JP6851315B2 - 金属酸化物粒子及びその生成方法 - Google Patents
金属酸化物粒子及びその生成方法 Download PDFInfo
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- JP6851315B2 JP6851315B2 JP2017547553A JP2017547553A JP6851315B2 JP 6851315 B2 JP6851315 B2 JP 6851315B2 JP 2017547553 A JP2017547553 A JP 2017547553A JP 2017547553 A JP2017547553 A JP 2017547553A JP 6851315 B2 JP6851315 B2 JP 6851315B2
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 77
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- 239000000956 alloy Substances 0.000 claims description 77
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium(II) oxide Chemical compound [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 52
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- 239000011572 manganese Substances 0.000 claims description 21
- 238000002844 melting Methods 0.000 claims description 18
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 14
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- 238000007254 oxidation reaction Methods 0.000 claims description 13
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- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 12
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- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 3
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 5
- 150000007513 acids Chemical class 0.000 description 5
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 3
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
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- 239000010419 fine particle Substances 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 2
- 235000013980 iron oxide Nutrition 0.000 description 2
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- 150000007522 mineralic acids Chemical class 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N nitrate group Chemical group [N+](=O)([O-])[O-] NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
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- AKFOHAJXLDHIEH-SNVBAGLBSA-N (3r)-3-(cyclobutanecarbonyloxy)-4-(trimethylazaniumyl)butanoate Chemical compound C[N+](C)(C)C[C@@H](CC([O-])=O)OC(=O)C1CCC1 AKFOHAJXLDHIEH-SNVBAGLBSA-N 0.000 description 1
- 241001061225 Arcos Species 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910000914 Mn alloy Inorganic materials 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 238000000184 acid digestion Methods 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- 239000003054 catalyst Substances 0.000 description 1
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- 238000012993 chemical processing Methods 0.000 description 1
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- 239000010941 cobalt Substances 0.000 description 1
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- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
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- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
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- 150000002500 ions Chemical class 0.000 description 1
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- IPJKJLXEVHOKSE-UHFFFAOYSA-L manganese dihydroxide Chemical compound [OH-].[OH-].[Mn+2] IPJKJLXEVHOKSE-UHFFFAOYSA-L 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- KELHQGOVULCJSG-UHFFFAOYSA-N n,n-dimethyl-1-(5-methylfuran-2-yl)ethane-1,2-diamine Chemical compound CN(C)C(CN)C1=CC=C(C)O1 KELHQGOVULCJSG-UHFFFAOYSA-N 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
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- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
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- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 230000037361 pathway Effects 0.000 description 1
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- 239000011164 primary particle Substances 0.000 description 1
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
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- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
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- 239000011882 ultra-fine particle Substances 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
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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
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1236—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching
- C22B34/124—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching using acidic solutions or liquors
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
- C01B13/32—Methods for preparing oxides or hydroxides in general by oxidation or hydrolysis of elements or compounds in the liquid or solid state or in non-aqueous solution, e.g. sol-gel process
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G1/00—Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general
- C01G1/02—Oxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
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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
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C22/00—Alloys based on manganese
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
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- C01P2006/12—Surface area
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Description
●「第1の金属(複数可)」と称される1つまたは少数の金属と、
●「第2の金属」と称される第2の金属と、を含む合金を使用する。
1.第2の金属を前駆体合金から除去すること。
2.第1の金属を完全に酸化して金属酸化物サブミクロン(ナノ)粒子にすること。
−第1の金属と第2の金属との合金を提供または形成することと、
−合金を熱処理に供して、ある特定の相組成物を固定することと、
−熱処理された合金を、第2の金属を浸出(除去)し、かつ第1の金属を完全に酸化するのに有効な浸出剤に供することにより、第1の金属酸化物を凝集ナノ粒子の形態で残すことと、
−浸出剤を除去して、第1の金属酸化物を残すことと、を含む。
●第1の金属(複数可)と第2の金属との合金を提供または形成することと、
●合金を熱処理操作に供することと、
●合金を、第2の金属を浸出し、かつ第1の金属(複数可)を酸化するのに有効な浸出剤に供することにより、第1の金属(複数可)の金属酸化物サブミクロン粒子を形成することと、
●浸出剤を除去して、第1の金属(複数可)の金属酸化物サブミクロン粒子を残すことと、を含む。
●第1の金属(複数可)と第2の金属との合金を提供または形成することと、
●合金を、第2の金属を浸出し、かつ第1の金属(複数可)を酸化するのに有効な浸出剤に供することにより、第1の金属(複数可)の金属酸化物サブミクロン粒子を形成することと、
●浸出剤を除去して、第1の金属(複数可)の金属酸化物サブミクロン粒子を残すことと、を含む。
一実施形態では、本発明は、金属酸化物粒子の粒径が3nm〜200nmの範囲であり、粒子の比表面積が70m2/gを超える、金属酸化物粒子を提供する。
一実施形態では、本発明は、1つ以上の第1の金属(複数可)のサブミクロン金属酸化物粒子を生成する方法を提供し、本方法は、
●第1の金属(複数可)と第2の金属との合金を提供または形成することと、
●任意に、合金を熱処理操作に供することと、
●合金を、第2の金属を浸出し、かつ第1の金属(複数可)を酸化するのに有効な浸出剤に供することにより、第1の金属(複数可)の金属酸化物サブミクロン粒子を形成することと、
●浸出剤を除去して、第1の金属(複数可)の金属酸化物サブミクロン粒子を残すことと、を含む。
1.体心立方(BCC)結晶構造を有するδMn固溶体。
2.面心立方(FCC)結晶構造を有するγMn固溶体。
3.複雑立方結晶構造を有するβMn固溶体。
4.複雑心立方(CBCC)結晶構造を有するαMn固溶体。
5.明確に特定されていない結晶構造を有するTiMn4またはTi2Mn9(異なる参考文献による)金属間化合物。
ナノサイズ粒子を含む酸化チタン粉末の調製
酸化チタン粉末の製造に使用される出発Mn−Ti合金を溶融するために、以下の原材料を使用した。
1.チタン:粉末形態、45ミクロン未満、純度99.98%、Sigma−Aldrich(製品番号366994)製。
2.マンガン:顆粒形態、粒径0.8〜12mm、純度99.98%、Alpha−Aesar製。
Ti合金粉末のマイクロ波支援酸消化及びICP−AES分析
酸化チタン粒子を含む生成物試料を、金属含有量について試験した。結果を以下の表に要約する。
試料バッチ(約20mg)を7mLのHNO3(65%)及び3mLのH2SO4(98%)中で消化した。消化を、高温及び高圧で「Discover」試料消化システム(CEM、USA)を使用して石英容器内で行った。これらの容器を冷却し、体積を脱イオン水で最大25mLにした。試料を完全に溶解した。元素濃度を、End−On−Plasma ICP−AESモデル「ARCOS」(Spectro GMBH,Germany)を使用して透明な溶液中で測定した。測定結果をICP(Merck)の標準で較正した。継続較正検証標準を測定して、計器の安定性を確認した。
Claims (24)
- 1つ以上の第1の金属(複数可)のサブミクロン金属酸化物粒子を生成する方法であって、
●前記第1の金属(複数可)と第2の金属との合金を提供または形成することと、
●前記合金を、前記第2の金属を浸出し、かつ前記第1の金属(複数可)を酸化するのに有効な浸出剤に供することにより、前記第1の金属(複数可)の金属酸化物サブミクロン粒子を形成することと、
●前記浸出剤を除去して、前記第1の金属(複数可)の前記金属酸化物サブミクロン粒子を残すことと、を含み、
前記第1の金属(複数可)は、Ti、Fe、Zr、Hf、Cu、Co、Cr、Ni、Mo、La、Nb、Ta、W、V、及びそれらの組み合わせからなる群から選択され、かつ前記第2の金属は、Mn、Mg、Zn、Ca、Ba、Sn、Pb、Be、Cd、Tl、B、及びそれらの組み合わせから選択される、方法。 - 前記合金を熱処理操作に供するステップをさらに含む、請求項1に記載の方法。
- 前記熱処理操作に供するステップが、合金を前記提供または形成する前記ステップの後であり、かつ前記合金を浸出剤に供する前記ステップの前に行われる、請求項2に記載の方法。
- 前記浸出剤の除去後に前記第1の金属(複数可)酸化物粒子をすすいで乾燥させることをさらに含む、請求項1に記載の方法。
- 前記すすぎが水中で行われ、前記水をすすいだ後にpHの観点で中性になったときに停止される、請求項4に記載の方法。
- 前記熱処理操作に供するステップが前記合金の均一相(複数可)を形成し、それから前記第2の金属が除去され、前記第1の金属(複数可)が前記浸出剤によって酸化される、請求項2に記載の方法。
- 前記合金が、1〜50重量%の前記第1の金属(複数可)及び50〜99重量%の前記第2の金属を含む、請求項1に記載の方法。
- 前記熱処理操作に供するステップ後に、前記合金が表面清浄操作を受ける、請求項2に記載の方法。
- 前記合金が、前記熱処理操作に供するステップ前または前記浸出前に粉砕操作に供される、請求項2に記載の方法。
- 前記浸出操作に使用される前記浸出剤が、前記第1の金属(複数可)の酸化を可能にする、請求項1に記載の方法。
- 前記浸出剤が少なくとも2つの化学剤を含む、請求項1に記載の方法。
- 前記化学剤のうちの第1の化学剤が前記第1の金属(複数可)の酸化に作用し、前記化学剤のうちの第2の化学剤が前記第2の金属の浸出に作用するか、または前記少なくとも2つの化学剤が前記第1の金属(複数可)の酸化及び前記第2の金属の浸出の両方に作用する、請求項11に記載の方法。
- 前記第1の金属(複数可)の酸化が均一金属酸化物粒子構造をもたらす、請求項10に記載の方法。
- 前記第1の金属がチタンであり、前記第2の金属がマンガンである、請求項1に記載の方法。
- 前記浸出剤が少なくとも1つの酸を含む、請求項1に記載の方法。
- 前記浸出剤が、3〜50%の範囲の濃度で、硝酸(HNO3)、塩酸(HCl)、硫酸(H2SO4)、またはそれらの組み合わせを含む、請求項15に記載の方法。
- 前記金属酸化物が、前記浸出及び前記すすぎ後に、脱水及び焼きなましのために加熱ステップを受ける、請求項4に記載の方法。
- 前記第1の金属がチタンであり、前記第2の金属がマンガンであり、前記浸出剤が硝酸(HNO3)を含む、請求項1に記載の方法。
- 前記金属酸化物粒子の結晶構造が、二酸化チタン(TiO2)であるか、または二酸化チタンと他の種類の酸化チタン(TiO)との混合体である、請求項1に記載の方法。
- 最終酸化チタン粒子の比表面積が70m2/gを超える、請求項1に記載の方法。
- 合金の前記形成が、前記第1の金属の固体を前記第2の金属の固体と混合することと、溶融物が形成されるように前記混合物を加熱することと、を含む、請求項1に記載の方法。
- 前記混合物が8%のTi及び92%のMnを含む、請求項21に記載の方法。
- 前記混合物に使用される前記第1の金属及び前記第2の金属が、粉末形態、顆粒形態、またはそれらの組み合わせである、請求項21に記載の方法。
- 溶融物を形成するための前記加熱が、希ガス保護雰囲気下で、溶融炉内で行われる、請求項21に記載の方法。
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