TWI242538B - Method for manufacturing crystalline powder of a lithium and vanadium oxide - Google Patents
Method for manufacturing crystalline powder of a lithium and vanadium oxide Download PDFInfo
- Publication number
- TWI242538B TWI242538B TW092123452A TW92123452A TWI242538B TW I242538 B TWI242538 B TW I242538B TW 092123452 A TW092123452 A TW 092123452A TW 92123452 A TW92123452 A TW 92123452A TW I242538 B TWI242538 B TW I242538B
- Authority
- TW
- Taiwan
- Prior art keywords
- lithium
- powder
- crystalline powder
- paste
- temperature
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000000843 powder Substances 0.000 title claims abstract description 18
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 8
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 8
- 229910001947 lithium oxide Inorganic materials 0.000 title abstract description 5
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 title abstract description 3
- 229910001935 vanadium oxide Inorganic materials 0.000 title abstract description 3
- 239000002243 precursor Substances 0.000 claims abstract description 7
- 239000000725 suspension Substances 0.000 claims abstract description 6
- 239000007900 aqueous suspension Substances 0.000 claims abstract description 4
- 239000002131 composite material Substances 0.000 claims abstract description 4
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 4
- 238000001354 calcination Methods 0.000 claims abstract 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 4
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 4
- FZRNJOXQNWVMIH-UHFFFAOYSA-N lithium;hydrate Chemical compound [Li].O FZRNJOXQNWVMIH-UHFFFAOYSA-N 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 229910007086 Li1+xV3O8 Inorganic materials 0.000 abstract 2
- 229910003206 NH4VO3 Inorganic materials 0.000 abstract 1
- 230000018044 dehydration Effects 0.000 abstract 1
- 238000006297 dehydration reaction Methods 0.000 abstract 1
- 239000002904 solvent Substances 0.000 description 8
- 239000007787 solid Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- ALTWGIIQPLQAAM-UHFFFAOYSA-N metavanadate Chemical compound [O-][V](=O)=O ALTWGIIQPLQAAM-UHFFFAOYSA-N 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000002178 crystalline material Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 150000003682 vanadium compounds Chemical class 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002642 lithium compounds Chemical class 0.000 description 1
- 229910000103 lithium hydride Inorganic materials 0.000 description 1
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000008247 solid mixture Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000000844 transformation Methods 0.000 description 1
- WQEVDHBJGNOKKO-UHFFFAOYSA-K vanadic acid Chemical compound O[V](O)(O)=O WQEVDHBJGNOKKO-UHFFFAOYSA-K 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Secondary Cells (AREA)
Description
1242538 (1) 玖、發明說明 【發明所屬之技術領域】 本發明係關於一種製造式LiI+xV3〇8(x在0與0.2之 間）之鋰和釩複合氧化物之晶體粉末的方法。此產品可特 別用來製造可充電型鋰電池所用電極。 【先前技術】 現存所有用來合成Li1+xV3 08複合氧化物的方法都採 用釩化合物在鋰鹽上的反應。彼等之不同在於彼等是否有 用到溶劑。 以水爲溶劑導致凝膠之形成經揭示於專利U S 5 0 3 9 5 8 2 (?13丁01八）之中。這種凝膠係以1^〇^1與¥2 05花費24小 時以上而得’且難以過濾及乾燥。專利 U S 6 1 7 7 1 3 0 (FREY)述及一種氧化鋰與釩酸的水溶液，係以偏釩酸銨 (MVA)通過樹脂上而製備。將此溶液乾燥且將其殘留物再 溶解於有機溶劑中以產生一種可用來塗佈光學品質薄層的 產品。例如，在美國專利 5 549 8 8 0 (KOKS BANG)與專利 申請 WO 0 1 /22 5 07 (3 M)中提及有機溶劑之使用，但在產 業階段中有環境與安全上的問題。不論溶劑種類爲何，習 知方法都沒有連續性且受限於過濾步驟。 不用溶劑，在固體混合物上操作是可能的。最後化合 物係經由熔化該混合物如美國專利 5 0 1 3 62 0 (Bridgestone)及 A.D. WADSLEY, Acta Cryst. 1 0 ( 1 9 5 7) 2 6 1的文章中所述者，或在稍低於熔點下轉化如美國專利 -5- 1242538 (2) ^ 5 5 20903 (CHANG)中所述而得到者。此等方法會造成熔融 或燒結塊中的材料在運輸與硏磨上的問題。 美國專利 6136476 (Hydro-Quebec and 3M)揭示鋰化 合物與釩化合物之乾粉的混料，噴氣硏磨，及在低於熔化 溫度之下加熱。該方法使得在所有製造步驟中可良好地控 制大小等級，且步驟數目相當有限。 不過’固體方法與溶劑使用比較之下有數個缺點，其 可使藥劑較密切混合而致更有效率之反應，及更容易的實 施。當合成晶體材料時，溶劑合後的結晶可在比固體方法 · 較爲低的溫度下進行，因此較爲方便且更經濟。最後，當 溶液中諸藥劑之一製得後，溶劑方法不需乾燥步驟。 - 本發明的目的是提供一種以幾近連續方式製造 -
Li 1+xV3〇8之晶體粉末的方法，其可以用有限數目的步驟 輕易地工業化，其中每一步驟之大小等級都可控制，且以 偏釩酸銨（MVA)與氫化鋰藥劑開始。 【發明內容】 · 本發明之目的係一種製造式Li】+xV3〇8(x在0與0.2 · 之間）複合鋰和釩氧化物之晶體粉末的方法，其包括： - - 從N H 0 3糊狀物與單水合氧化鋰粉末起始形成水 性懸浮液， - 將此懸浮液置於在2 0 0與6 0 0 ° C之間的溫度之熱 氣體流中予以連續脫水而形成大小等級在！ 〇到1 〇 〇微米 之間的先質之乾粉， -6 - 1242538 (3) - 在3 8 0到5 8 0 ° C之間的溫度鍛燒此先質以形成
Li1+xV 3 0 8晶體粉末。 本方法開始於將Μ V A糊狀物與單水合氧化鋰粉末置 入水性懸浮液，其質量比爲可以得到產生L i ]+ x V 3 0 8 (X在 0與0.2之間）所需的Li/V化學計量。固體對總質量之比 係在4 0到6 0 %之間。 溶劑的使用促成較固體方法更密切的藥劑混合且更容 易實施。再者，在合成一單相晶體材料的特殊情況中，該 溶劑方法需要比固體方法較爲低的結晶溫度因而較低的能 源成本。 與美國專利 6 1 3 6 4 7 6中所述方法比較，使用水性溶 劑具備技術-經濟優點。MVA的無機合成程序是在燒結或 乾燥前，Μ V A —定要以在潮濕狀態製得。乾燥步驟沒有 用且可能將MVA (潮濕的糊狀物或懸浮液）直接注入製 程，不論使用之Μ V A是否爲超純度或爲採礦作業中之釩 萃取所用濕式冶金循環中之中間V 2 Ο 5產物。此外，如果 結合會消耗氨的釩濕式冶金作業時，則這種氣體流出物的 回收可能有經濟上與環保上的吸引力。 將如此所得之懸浮液在中性氣圍，例如氮氣圍中且在 20到90 ° C之間持續攪拌半小時到24小時，直到其加到 熱氣體噴霧器，例如 RIERA NADEU S.A.公司製造之 RINAJET噴霧器之內爲止。由此儀器噴出的熱氣體之強 烈渦流（2 50-600 ° C )使得固態成品瞬間脫水且製成乾粉 形式，大小等級在1 0到1 00微米之間的最終產物之先質 -7-
Claims (1)
1242538 (1) 拾、申請專利範圍 1.一種製造式1^1+^3〇8(其中>(介於〇與0.2之間）之 鋰和釩複合氧化物之晶體粉末的方法，其包括： - 從NH4V03糊狀物與單水合氧化鋰粉末起始形成水性 懸浮液， - 將此懸浮液於2 0 0與600 ° C之間溫度之熱氣體流中予 以連續脫水，而形成大小等級在1 〇到1 〇〇微米之間的先 質乾粉， - 在介於3 8 0到5 8 0 ° C之間的溫度鍛燒此先質’以形成 Li1+xV 3 0 8的晶體粉末。 2 ·如申請專利範圍第1項之方法，其中該懸浮液在注 入到熱氣體流之前係先經攪拌。 3 ·如申請專利範圍第1項之方法，其中該最終產物之 大小等級係在介於1 0到1 〇 〇微米之間。 4 ·如申請專利範圍第1至3項中任一項之方法，其中 該NHaVO3糊狀物係爲藉由使VOCI3與NH4〇H反應所製 得之高純度糊狀物。 -11 -
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR0211370A FR2844508B1 (fr) | 2002-09-13 | 2002-09-13 | Procede de fabrication de poudre cristalline d'oxyde de lithium et de vanadium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| TW200412328A TW200412328A (en) | 2004-07-16 |
| TWI242538B true TWI242538B (en) | 2005-11-01 |
Family
ID=31897365
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| TW092123452A TWI242538B (en) | 2002-09-13 | 2003-08-26 | Method for manufacturing crystalline powder of a lithium and vanadium oxide |
Country Status (15)
| Country | Link |
|---|---|
| US (1) | US20060039851A1 (zh) |
| EP (1) | EP1537049B1 (zh) |
| JP (1) | JP2006507202A (zh) |
| CN (1) | CN1317196C (zh) |
| AR (1) | AR041063A1 (zh) |
| AT (1) | ATE336465T1 (zh) |
| AU (1) | AU2003278295A1 (zh) |
| CA (1) | CA2495702A1 (zh) |
| DE (1) | DE60307655T2 (zh) |
| ES (1) | ES2265589T3 (zh) |
| FR (1) | FR2844508B1 (zh) |
| RU (1) | RU2005110946A (zh) |
| TW (1) | TWI242538B (zh) |
| WO (1) | WO2004024631A1 (zh) |
| ZA (1) | ZA200501931B (zh) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2866641B1 (fr) | 2004-02-23 | 2006-06-16 | Batscap Sa | Procede de preparation d'un oxyde de lithium et de vanadium |
| FR2876997B1 (fr) * | 2004-10-22 | 2007-01-19 | Batscap Sa | Oxyde de lithium et de vanadium, procede pour sa preparation |
| CN100436326C (zh) * | 2006-10-13 | 2008-11-26 | 福建师范大学 | 一种用于锂离子电池正极材料的锂钒氧化物的制备方法 |
| TW201002623A (en) * | 2008-05-30 | 2010-01-16 | Basf Se | Process for preparing lithium vanadium oxides and their use as cathode material |
| TW201107242A (en) | 2009-05-27 | 2011-03-01 | Conocophillips Co | Methods of making lithium vanadium oxide powders and uses of the powders |
| CN101916852B (zh) * | 2009-11-29 | 2013-02-20 | 宁波大学 | 一种负衰减系数锂离子电池正极材料钒酸锂的制备方法 |
| CN103236533A (zh) * | 2013-04-22 | 2013-08-07 | 中南大学 | 一种锂离子电池用钒酸钾纳米带材料及其制备方法 |
| US20170141245A1 (en) * | 2015-11-12 | 2017-05-18 | E I Du Pont De Nemours And Company | Conductive paste composition and semiconductor devices made therewith |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| IT1231750B (it) | 1989-05-12 | 1991-12-21 | Consiglio Nazionale Ricerche | Accumulatori al litio ad alta energia e potenza e relativo metodo di produzione |
| JPH02288068A (ja) | 1989-04-26 | 1990-11-28 | Bridgestone Corp | 非水電解液二次電池 |
| US5512214A (en) * | 1993-03-30 | 1996-04-30 | Koksbang; Rene | Lithium battery electrode compositions |
| US5520903A (en) | 1993-11-15 | 1996-05-28 | Chang; On K. | Method of making lithium metal oxide cathode active material |
| US5549880A (en) | 1994-03-31 | 1996-08-27 | Koksbang; Rene | Method of making lithium-vanadium-oxide active material |
| US6177130B1 (en) | 1998-03-02 | 2001-01-23 | Minnesota Mining And Manufacturing Company | Method of preparing lithiated vanadium oxide-coated substrates of optical quality |
| SG86325A1 (en) * | 1998-06-23 | 2002-02-19 | Univ Singapore | Method for preparing a cathode material and electrochemical cell having a cathode based on same |
| US6136476A (en) | 1999-01-29 | 2000-10-24 | Hydro-Quebec Corporation | Methods for making lithium vanadium oxide electrode materials |
| US6322928B1 (en) | 1999-09-23 | 2001-11-27 | 3M Innovative Properties Company | Modified lithium vanadium oxide electrode materials and products |
-
2002
- 2002-09-13 FR FR0211370A patent/FR2844508B1/fr not_active Expired - Fee Related
-
2003
- 2003-08-26 TW TW092123452A patent/TWI242538B/zh not_active IP Right Cessation
- 2003-08-27 AR ARP030103095A patent/AR041063A1/es unknown
- 2003-09-10 CA CA002495702A patent/CA2495702A1/fr not_active Abandoned
- 2003-09-10 JP JP2004535593A patent/JP2006507202A/ja active Pending
- 2003-09-10 ES ES03769604T patent/ES2265589T3/es not_active Expired - Lifetime
- 2003-09-10 RU RU2005110946/15A patent/RU2005110946A/ru not_active Application Discontinuation
- 2003-09-10 US US10/527,595 patent/US20060039851A1/en not_active Abandoned
- 2003-09-10 AU AU2003278295A patent/AU2003278295A1/en not_active Abandoned
- 2003-09-10 AT AT03769604T patent/ATE336465T1/de not_active IP Right Cessation
- 2003-09-10 CN CNB038217058A patent/CN1317196C/zh not_active Expired - Fee Related
- 2003-09-10 WO PCT/FR2003/002685 patent/WO2004024631A1/fr not_active Ceased
- 2003-09-10 EP EP03769604A patent/EP1537049B1/fr not_active Expired - Lifetime
- 2003-09-10 DE DE60307655T patent/DE60307655T2/de not_active Expired - Fee Related
-
2005
- 2005-03-07 ZA ZA200501931A patent/ZA200501931B/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| US20060039851A1 (en) | 2006-02-23 |
| AU2003278295A1 (en) | 2004-04-30 |
| DE60307655T2 (de) | 2007-08-16 |
| TW200412328A (en) | 2004-07-16 |
| FR2844508A1 (fr) | 2004-03-19 |
| ZA200501931B (en) | 2006-05-31 |
| EP1537049B1 (fr) | 2006-08-16 |
| CA2495702A1 (fr) | 2004-03-25 |
| DE60307655D1 (de) | 2006-09-28 |
| FR2844508B1 (fr) | 2005-12-16 |
| HK1081516A1 (zh) | 2006-05-19 |
| CN1317196C (zh) | 2007-05-23 |
| JP2006507202A (ja) | 2006-03-02 |
| ES2265589T3 (es) | 2007-02-16 |
| RU2005110946A (ru) | 2005-09-20 |
| WO2004024631A1 (fr) | 2004-03-25 |
| WO2004024631A8 (fr) | 2005-04-28 |
| CN1681739A (zh) | 2005-10-12 |
| EP1537049A1 (fr) | 2005-06-08 |
| ATE336465T1 (de) | 2006-09-15 |
| AR041063A1 (es) | 2005-04-27 |
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