WO2009064265A1 - Method and devices for producing air sensitive electrode materials for lithium ion battery applications - Google Patents
Method and devices for producing air sensitive electrode materials for lithium ion battery applications Download PDFInfo
- Publication number
- WO2009064265A1 WO2009064265A1 PCT/US2007/023784 US2007023784W WO2009064265A1 WO 2009064265 A1 WO2009064265 A1 WO 2009064265A1 US 2007023784 W US2007023784 W US 2007023784W WO 2009064265 A1 WO2009064265 A1 WO 2009064265A1
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- WIPO (PCT)
- Prior art keywords
- materials
- synthesizing process
- vessel
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- synthesizing
- Prior art date
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
-
- 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
Definitions
- the present invention is concerned with reaction chambers to be utilized for the mass production of air sensitive materials, especially for the synthesis of electrode materials for lithium batteries.
- Oxidation and reduction reactions are commonly utilized for the synthesis of inorganic crystalline materials. This is especially true for the synthesis of electrode materials for Li-ion batteries including cathode and anode materials.
- cathode materials such as lithium cobalt oxide, lithium nickel oxide, lithium manganese oxide and the mixed oxides are synthesized under oxidative environments. These materials are more readily obtainable since control of an oxidative heat treatment environment (e.g. heat treatment in open air environment) is not difficult. In contrast, a reductive environment is less feasible since control of a reductive heat treatment atmosphere is difficult.
- the difficulty stems from the fact that during the heat treatment steps of the synthesis, especially at elevated temperatures (e.g.
- the present invention is a unit, for use within a furnace absent a controlled atmosphere, in a synthesizing process for synthesizing precursors to form a synthesized product at elevated temperatures.
- the unit has a vessel, having at least one opening, for containing materials of the synthesizing process, and a solid reductive material, wherein the materials of the synthesizing process are separated from the atmosphere of the furnace by either the vessel or the reductive material.
- Figs. l(a) and l(b) are illustrations of a first embodiment of the unit of the invention.
- Figs. l(c) and l(d) are illustrations of a second embodiment of the unit of the invention.
- Fig. l(e) is an illustration of a third embodiment of the unit of the invention.
- Fig. 2(a) is an illustration of units of the first and/or second embodiments in a furnace for carrying out a synthesizing process
- Fig. 2(b) is an illustration of units of the third embodiment in a furnace for carrying out a synthesizing process
- Fig. 3 is a graph of an x-ray diffraction pattern for a representative sample of a synthesized electrode material prepared using units of the invention
- Fig. 4 is a graph for showing battery test data for the same material as in Fig. 3;
- Fig. 5 is a graph of x-ray diffraction patterns for 5 similar synthesized electrode materials prepared using units of the invention.
- Fig. 6 is a graph for showing battery test data for 10 similar synthesized electrode materials prepared using units of the invention.
- Figs. l(a) - l(e) show schematic diagrams of individually sealed units (ISU) containing materials that are subjected to the synthesizing heat treatments. Designs of furnaces that contain the ISUs of different geometries are shown in Figs. 2(a) and 2(b).
- ISU individually sealed units
- the ISU 1 is a vessel having one end 2 completely sealed while the other end 3 is open to the atmosphere.
- Precursors to be synthesized to form an electrode material are contained at 4.
- the precursors, intermediate products, and resulting material of the synthesizing process are referred to as materials of the synthesizing process throughout the description.
- the materials of the synthesizing process, contained at 4 are protected from the atmosphere of the furnace, into which ISUs are placed for heating, by either the material of the vessel 1, or a solid reductive material layer 5 that limits the permeation of air from the furnace atmosphere. It should be mentioned that since the reductive material (e.g.
- the porosity of the reductive material layer would allow the permeation of any gas by-product released from the material being synthesized, to the atmosphere.
- the gas by-product or the oxidation of the reductive material would generate gas and keep the pressure within the ISU positive, compared to the atmosphere.
- a decrease of the porosity of the reductive material layer would ensure separation from the atmosphere.
- each ISU of a second embodiment is a vessel 1 having both ends 6 open to the environment.
- Precursors to be synthesized to form an electrode material are contained at 4.
- the materials of the synthesizing process, contained at 4 are protected from the atmosphere of the furnace, into which ISUs are placed for heating, by solid reductive material layers 5 that limit the permeation of air from the furnace atmosphere.
- the solid reductive material is usually porous to allow permeation of any gases resulting from the synthesizing process.
- a divider 11 can be used to separate the reductive material 5 from the material 4 of the synthesizing process.
- the divider preferably is inert to the materials being separated and porous to any gases being generated.
- a high-temperature durable glass fiber packing can be used to hold all of the materials in the vessels .
- FIG. l(e) Similar characteristics can be observed in a third embodiment of an ISU shown in Fig. l(e). From Fig. l(e), it can be seen that the materials to be synthesized 4 are contained in a crucible 8. The path of airflow from any open side of a vessel 9 is controlled by the presence of reductive material 10. A bottom of the crucible separates the reductive material from the materials of the synthesizing process. A tray 12 facilitates handling of the unit. Vessel 9 is not sealed tightly against tray 12 in order that gases can flow freely to or from the reductive material, as shown at 18.
- Figs. 2(a) and 2(b) show the various embodiments of the invention as utilized in a furnace to carry out the synthesizing process.
- FIG. 2(a) first embodiments and/or second embodiments are shown in furnace 13. Heating elements of the furnace are shown at 14.
- Fig. 2(b) four units of the third embodiment of the invention are shown at 15 in furnace 16. Heating elements of the furnace are shown at 17. As mentioned above, the furnaces are not required to be sealed and a controlled inert or reducing environment is not necessary.
- An ISU includes a space that contains the materials being subjected to the synthesizing heat treatment; b. An ISU includes a space that contains the reductive material; c. The reductive material is placed in the vessel in a manner as:
- Uncontrolled atmosphere/reductive material/synthesized material (Figs. l(a) and l(b)), or uncontrolled atmosphere/reductive material/synthesized material/ reductive material/uncontrolled atmosphere (Figs. l(c) and l(d)); d.
- the reductive material can be placed on top of the synthesized material as shown in Figs. l(a) -l(d) or somewhere else in contact with the outer atmosphere as shown in
- the ISU can dissipate gas generated by the synthesizing reaction.
- the flow of gases is from the materials of the synthesizing process, through the reductive material to the uncontrolled atmosphere, or the reverse of same.
- the flow of gases is from the materials of the synthesizing process, through the separator, through the reductive material to the uncontrolled atmosphere, or the reverse of the same.
- the flow of gases is from the materials of the synthesizing process, through the separation between the crucible and the vessel, through the reductive material to the uncontrolled atmosphere, or the reverse of same.
- the as-prepared material was then subjected to grinding and ball milling for about 12 hours.
- the ground powdery materials was then loaded into several ISUs as shown in Fig. l(a) with the addition of a carbonaceous material placed directly on top of the ground powdery material for heat treatment.
- the carbonaceous material can be placed directly on top of the synthesized material or separated by a thin layer of porous glass fiber fabrics or other inert plate.
- the ISUs were then placed in a furnace as shown in Fig. 2(a).
- the heat treatment was conducted at 65O 0 C for 24 hours resulting in the synthesized material. After the heat treatment step, slight grinding and sieving were conducted on the synthesized material. The post-heat treated materials were then ready for further tests, as will be described below.
- ISUs The utilization of ISUs is not limited to the synthesis of lithium iron phosphate, or limited to the choice of starting materials and precursor processing steps described for the synthesis of lithium iron phosphate of the present example.
- X-ray diffraction pattern data of the synthesized material is shown in Fig. 3. It is observed that phase pure material was obtained using the processing methods and devices presented in this example, without the use and control of an inert gas, such as nitrogen or argon. Battery test data (obtained using a three electrode design test battery and lithium is utilized as the reference electrode) are shown in Fig. 4. From Fig. 4 it can be seen that the capacity is high during the first charge-discharge cycle ( ⁇ C/5 rate, 0.23mA/cm 2 ). The material synthesized in the present case is comparable or superior to the prior art material disclosed in U.S. Patent No. 6,723,470, which was obtained using an inert atmosphere as a heat treatment environment.
- the devices of the present invention provide the following advantages. There is no need for the use of an inert gas in the furnace, such as nitrogen or argon, or forming gas (nitrogen plus hydrogen), thus a completely sealed furnace is not required.
- the ISUs are semi-open to the atmosphere of the furnace, thus sealing of the ISUs is not difficult. There is a short thermal diffusion distances from the heat source to the material being synthesized.
- the reductive material such as carbon black or carbonaceous materials for air permeation prevention, even if a small amount of air permeation occurs during heat treatment, oxidation of the carbonaceous material prevents further oxidation of the material being synthesized.
- the reductive material can be porous so to allow the dissipation of gas produced by the materials that are subjected to the heat treatment.
- the depth of the ISUs shown in Fig. l(a) and l(b) are adjustable for the prevention of oxidation, for example a longer depth would give a better-isolated environment.
- the geometry of the ISUs is flexible to accommodate the design of the furnaces, such as shown in Figs. 2(a) and 2(b).
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Furnace Charging Or Discharging (AREA)
Abstract
Description
Claims
Priority Applications (7)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CA2705260A CA2705260C (en) | 2007-11-14 | 2007-11-14 | Method and devices for producing air sensitive electrode materials for lithium ion battery applications |
CN200780101498A CN101855371A (en) | 2007-11-14 | 2007-11-14 | Method and devices for producing air sensitive electrode materials for lithium ion battery applications |
JP2010533999A JP5795164B2 (en) | 2007-11-14 | 2007-11-14 | Method and apparatus for manufacturing an air sensitive electrode material for application in a lithium ion battery |
EP07861961.6A EP2209925A4 (en) | 2007-11-14 | 2007-11-14 | Method and devices for producing air sensitive electrode materials for lithium ion battery applications |
PCT/US2007/023784 WO2009064265A1 (en) | 2007-11-14 | 2007-11-14 | Method and devices for producing air sensitive electrode materials for lithium ion battery applications |
KR1020107012698A KR101188069B1 (en) | 2007-11-14 | 2007-11-14 | Method and devices for producing air sensitive electrode materials for lithium ion battery applications |
TW097142619A TWI427028B (en) | 2007-11-14 | 2008-11-05 | Method and devices for producing air sensitive electrode materials for lithium ion battery applications |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
PCT/US2007/023784 WO2009064265A1 (en) | 2007-11-14 | 2007-11-14 | Method and devices for producing air sensitive electrode materials for lithium ion battery applications |
Publications (1)
Publication Number | Publication Date |
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WO2009064265A1 true WO2009064265A1 (en) | 2009-05-22 |
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Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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PCT/US2007/023784 WO2009064265A1 (en) | 2007-11-14 | 2007-11-14 | Method and devices for producing air sensitive electrode materials for lithium ion battery applications |
Country Status (7)
Country | Link |
---|---|
EP (1) | EP2209925A4 (en) |
JP (1) | JP5795164B2 (en) |
KR (1) | KR101188069B1 (en) |
CN (1) | CN101855371A (en) |
CA (1) | CA2705260C (en) |
TW (1) | TWI427028B (en) |
WO (1) | WO2009064265A1 (en) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2011249338A (en) * | 2010-05-27 | 2011-12-08 | Harmony Brother Co Ltd | Method for sintering lithium-containing electrode material |
JP2011258398A (en) * | 2010-06-09 | 2011-12-22 | Chin-Shin Green Energy Co Ltd | Method of sintering lithium containing electrode material |
WO2013109312A1 (en) * | 2012-01-19 | 2013-07-25 | Dow Global Technologies Llc | Article and method for venting a processing vessel |
US10041049B2 (en) | 2008-11-03 | 2018-08-07 | Janssen Vaccines & Prevention B.V. | Method for the production of adenoviral vectors |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP5181022B2 (en) * | 2007-07-31 | 2013-04-10 | ビーワイディー カンパニー リミテッド | Method for preparing lithium iron phosphate as positive electrode active material for lithium ion secondary battery |
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US20060119024A1 (en) * | 2003-07-25 | 2006-06-08 | Nippon Crucible Co., Ltd. | Molten-metal transferring ladle and molten-metal tapping method |
US7264767B2 (en) * | 2000-07-21 | 2007-09-04 | Norddeutsche Affinerie Aktiengesellschaft | Method and device for reducing the oxygen content of a copper melt |
US20070212606A1 (en) * | 2006-03-08 | 2007-09-13 | Chun-Chieh Chang | Cathode material for Li-ion battery applications |
US20070221122A1 (en) * | 2004-12-28 | 2007-09-27 | Matsushita Electric Industrial Co., Ltd. | Method for Producing Silicon Carbide (Sic) Single Crystal and Silicon Carbide (Sic) Single Crystal Obtained By Such Method |
Family Cites Families (7)
Publication number | Priority date | Publication date | Assignee | Title |
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JPH02176389A (en) * | 1988-12-28 | 1990-07-09 | Osaka Gas Co Ltd | Sintering of inorganic substance and crucible for sintering |
JPH11339798A (en) * | 1998-05-25 | 1999-12-10 | Kawasaki Steel Corp | Manufacture of carbon material for secondary battery negative electrode and obtained carbon material |
US6645452B1 (en) * | 2000-11-28 | 2003-11-11 | Valence Technology, Inc. | Methods of making lithium metal cathode active materials |
JP2007230784A (en) * | 2004-03-30 | 2007-09-13 | Agc Seimi Chemical Co Ltd | Manufacturing process of lithium-iron complex oxide |
JP4525474B2 (en) * | 2005-06-06 | 2010-08-18 | 株式会社豊田中央研究所 | Active material for lithium secondary battery and method for producing the same, lithium secondary battery |
JP4829557B2 (en) * | 2005-07-21 | 2011-12-07 | Agcセイミケミカル株式会社 | Method for producing lithium iron composite oxide |
JP2007035358A (en) * | 2005-07-25 | 2007-02-08 | Toyota Central Res & Dev Lab Inc | Positive electrode active substance, its manufacturing method and lithium ion secondary battery |
-
2007
- 2007-11-14 EP EP07861961.6A patent/EP2209925A4/en not_active Withdrawn
- 2007-11-14 CA CA2705260A patent/CA2705260C/en active Active
- 2007-11-14 KR KR1020107012698A patent/KR101188069B1/en active IP Right Grant
- 2007-11-14 WO PCT/US2007/023784 patent/WO2009064265A1/en active Application Filing
- 2007-11-14 JP JP2010533999A patent/JP5795164B2/en active Active
- 2007-11-14 CN CN200780101498A patent/CN101855371A/en active Pending
-
2008
- 2008-11-05 TW TW097142619A patent/TWI427028B/en active
Patent Citations (4)
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US7264767B2 (en) * | 2000-07-21 | 2007-09-04 | Norddeutsche Affinerie Aktiengesellschaft | Method and device for reducing the oxygen content of a copper melt |
US20060119024A1 (en) * | 2003-07-25 | 2006-06-08 | Nippon Crucible Co., Ltd. | Molten-metal transferring ladle and molten-metal tapping method |
US20070221122A1 (en) * | 2004-12-28 | 2007-09-27 | Matsushita Electric Industrial Co., Ltd. | Method for Producing Silicon Carbide (Sic) Single Crystal and Silicon Carbide (Sic) Single Crystal Obtained By Such Method |
US20070212606A1 (en) * | 2006-03-08 | 2007-09-13 | Chun-Chieh Chang | Cathode material for Li-ion battery applications |
Non-Patent Citations (1)
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US10041049B2 (en) | 2008-11-03 | 2018-08-07 | Janssen Vaccines & Prevention B.V. | Method for the production of adenoviral vectors |
JP2011249338A (en) * | 2010-05-27 | 2011-12-08 | Harmony Brother Co Ltd | Method for sintering lithium-containing electrode material |
JP2011258398A (en) * | 2010-06-09 | 2011-12-22 | Chin-Shin Green Energy Co Ltd | Method of sintering lithium containing electrode material |
WO2013109312A1 (en) * | 2012-01-19 | 2013-07-25 | Dow Global Technologies Llc | Article and method for venting a processing vessel |
CN104023816A (en) * | 2012-01-19 | 2014-09-03 | 陶氏环球技术有限责任公司 | Article and method for venting a processing vessel |
CN104023816B (en) * | 2012-01-19 | 2016-09-07 | 陶氏环球技术有限责任公司 | For goods and the method for vessel delivery will be processed |
Also Published As
Publication number | Publication date |
---|---|
CA2705260C (en) | 2013-08-06 |
JP5795164B2 (en) | 2015-10-14 |
TWI427028B (en) | 2014-02-21 |
KR20100112551A (en) | 2010-10-19 |
KR101188069B1 (en) | 2012-10-04 |
CN101855371A (en) | 2010-10-06 |
JP2011505536A (en) | 2011-02-24 |
CA2705260A1 (en) | 2009-05-22 |
EP2209925A4 (en) | 2017-11-22 |
EP2209925A1 (en) | 2010-07-28 |
TW200920691A (en) | 2009-05-16 |
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