CN103456925A - Rapid synthesis method of lithium cobaltous phosphate/carbon composite material for lithium ion battery through microwave - Google Patents

Rapid synthesis method of lithium cobaltous phosphate/carbon composite material for lithium ion battery through microwave Download PDF

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Publication number
CN103456925A
CN103456925A CN2013104019322A CN201310401932A CN103456925A CN 103456925 A CN103456925 A CN 103456925A CN 2013104019322 A CN2013104019322 A CN 2013104019322A CN 201310401932 A CN201310401932 A CN 201310401932A CN 103456925 A CN103456925 A CN 103456925A
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China
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lithium
salt
composite material
microwave
ion battery
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CN2013104019322A
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Chinese (zh)
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粟智
张玉
李珊珊
王帅
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Xinjiang Normal University
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Xinjiang Normal University
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

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Abstract

As a new anode material, LiCoPO4 has the advantages of potential high-energy density, low synthesis cost, environmental protection and the like. At present, particles are thinned and shapes of the particles are controlled through improvement of a preparation technology mainly so as to synthesize nano-scale LiCoPO4, the sizes of the particles and the tight bonding degree of the particles are changed through carbon coating and metal doping, and the diffusion path of Li+ is reduced, so that the conductivity of lithium ions is improved; therefore, the electrochemical performance of the material is greatly improved. According to the invention, synthetic raw materials including lithium dihydrogen phosphate (or by taking ammonium dihydrogen phosphate and lithium hydroxide or lithium salt, such as lithium acetate, or by taking phosphoric acid and lithium hydroxide or lithium salt as raw materials), basic cobaltous carbonate, conductive carbon black (or acetylene black or carbon nano-tubes or other carbon materials) are selected. Firstly, after ball-milling or stirring treatment of the raw materials, when the microwave power is in the range of 300-2000W, the synthesis time is 5-30 min, and the lithium cobaltous phosphate/carbon composite material for the lithium ion battery can be rapidly synthesized.

Description

The quick synthesizing lithium ion battery of microwave cobalt phosphate lithium/carbon composite material
Technical field
The present invention is based on and prepare the high performance lithium ion battery material and green synthesis process is starting point, developing Microwave Solid synthetic technology, select to take lithium salts (or lithium hydroxide), phosphoric acid (ammonium phosphate salt), cobalt salt, conductive carbon black (or acetylene black or glucose) to prepare the new method of lithium ion battery use cobalt phosphate lithium/carbon composite material for raw material.
Background technology
Synthetic and application study with transition metal phosphate crystallization functional material of the characteristics such as potential light, electricity, magnetic, catalysis is study hotspot nearly ten years.LiCoPO wherein 4be the positive electrode that the commercialization lithium-ions battery is used, its crystal has orderly olivine-type structure, belongs to rhombic system.LiCoPO 4the theoretical capacitance of positive electrode is 167 mAh/g, and security performance is good, with respect to about 4.8 V of lithium electrode electromotive force, is expected to become high power capacity of new generation, high-tension positive electrode.Positive electrode LiCoPO 4chemical property is limited by: the electronic conductivity of material is lower; Cycle performance has much room for improvement; The oxidation Decomposition of electrolyte during high voltage.By improving its preparation method, study new preparation technology, further investigated element doping, synthetic composite material and work out high pressure resistant, oxidation resistant electrolyte.Make LiCoPO once obtain in these areas progress 4chemical property is improved, that LiCoPO 4more wide application background will be had.The present invention proposes the quick synthesizing lithium ion battery of microwave cobalt phosphate lithium/carbon composite material, has optimized design technology, has greatly shortened the reaction time, and synthetic method and process economics, feasible, green, environmental protection and energy-conservation, have application value.
Summary of the invention
1. the quick synthesizing lithium ion battery of microwave cobalt phosphate lithium material, it is characterized in that take that lithium salts (or lithium hydroxide), phosphoric acid (ammonium phosphate salt), cobalt salt, conductive carbon black (or acetylene black or glucose) are raw material, adopt ball milling or stir process, adopt microwave radiation means, directly synthesizing lithium ion battery cobalt phosphate lithium/carbon composite material.
2. the present invention is characterized in that synthesis material comprises that take lithium salts (or lithium hydroxide), phosphoric acid (ammonium phosphate salt), cobalt salt, conductive carbon black (or acetylene black or glucose) is raw material, adopt ball milling or stir process, adopt the Microwave Solid method (to it is characterized in that minimum microwave power is 300W, generated time is no more than 30min), direct synthesizing lithium ion battery cobalt phosphate lithium/carbon composite material.
3. the present invention is characterized in that with lithium dihydrogen phosphate, (ammonium phosphate salt, cobalt salt, conductive carbon black (or acetylene black or glucose) prepare cobalt phosphate lithium as raw material, and its process comprises the steps: to take lithium salts (or lithium hydroxide), phosphoric acid
(1) (ammonium phosphate salt, cobalt salt, conductive carbon black (or acetylene black or glucose) are raw material, adopt as raw material, add appropriate water, are placed in the ball grinder ball milling, or are placed in reactor and stir 2-4h to take lithium salts (or lithium hydroxide), phosphoric acid.
(2) raw material stoving prepared is placed in reacting furnace, when minimum microwave power is 300W, reaction time 5-30min.
(3) will prepare material grinds standby.
the accompanying drawing explanation:
Fig. 1 is cobalt phosphate lithium/carbon composite material process chart for the quick synthesizing lithium ion battery of microwave.
Fig. 2 is that microwave power is 300W, and the reaction time is 10min, the X-ray diffractogram of the synthetic cobalt phosphate lithium/carbon composite material obtained.
Fig. 3 is that microwave power is 300W, and the reaction time is 10min, the infrared spectrogram of the synthetic cobalt phosphate lithium/carbon composite material obtained.
Fig. 4 is that microwave power is 300W, and the reaction time is 10min, the transmission electron microscope picture of the synthetic cobalt phosphate lithium/carbon composite material obtained.
specific embodiments
Get a certain amount of cobalt acetate, lithium carbonate, ammonium dihydrogen phosphate, glucose and water by metering score another name, put into flask stirring or ball milling 4h and obtain presoma, presoma is dried in rearmounted microwave oven, microwave power 300W is set, generated time 10min, then be cooled to room temperature standby.Its synthesis technique flow process is shown in Fig. 1, and the material X-ray diffraction spectrum is shown in Fig. 2, and infrared spectrum is shown in Fig. 3, and transmission electron microscope is shown in Fig. 4
4. according to described preparation technology, it is characterized in that optimum condition adopts carry out microwave radiation heating synthesizing lithium ion battery cobalt phosphate lithium/carbon composite material.Synthetic power 300-2000W, generated time 5-30min.
The above embodiment is only the preferred embodiments of the invention, should point out, for this area, is not breaking away under the prerequisite of creating conception of the present invention, and some distortion of making and improvement all belong to protection scope of the present invention.

Claims (5)

1. the quick synthesizing lithium ion battery of microwave cobalt phosphate lithium/carbon composite material, it is characterized in that take that lithium salts (or lithium hydroxide), phosphoric acid (ammonium phosphate salt), cobalt salt, conductive carbon black (or acetylene black or glucose) are raw material, at first adopt ball milling or stir process, then adopt the quick synthesizing lithium ion battery of microwave radiation means nickel phosphate lithium/carbon composite material.
2. method according to claim 1, is characterized in that synthesis material comprises phosphorus lithium salts (or lithium hydroxide), phosphoric acid (ammonium phosphate salt), cobalt salt, conductive carbon black (or acetylene black or glucose).
3. method according to claim 1, the minimum synthetic microwave power 300W of its feature.
4. method according to claim 1, is characterized in that generated time 5-30min.
5. it is characterized in that lithium salts (or lithium hydroxide), phosphoric acid (ammonium phosphate salt), cobalt salt, conductive carbon black (or acetylene black or glucose) are raw material, adopt microwave radiation means to prepare the cobalt phosphate lithium/carbon composite material, its process comprises the steps:
(1) take lithium salts (or lithium hydroxide), phosphoric acid (ammonium phosphate salt), cobalt salt, conductive carbon black (or acetylene black or glucose) is raw material, adopts as raw material, adds appropriate water, is placed in the ball grinder ball milling, or is placed in reactor and stirs 2-4h;
(2) raw material stoving prepared is placed in reacting furnace, when minimum microwave power is 300W, reaction time 5-30min;
(3) will prepare material grinds standby.
CN2013104019322A 2013-09-06 2013-09-06 Rapid synthesis method of lithium cobaltous phosphate/carbon composite material for lithium ion battery through microwave Pending CN103456925A (en)

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CN2013104019322A CN103456925A (en) 2013-09-06 2013-09-06 Rapid synthesis method of lithium cobaltous phosphate/carbon composite material for lithium ion battery through microwave

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105576204A (en) * 2015-12-23 2016-05-11 厦门大学 Graphene composite carbon-coated cobalt-lithium phosphate material and preparation methods and application thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105576204A (en) * 2015-12-23 2016-05-11 厦门大学 Graphene composite carbon-coated cobalt-lithium phosphate material and preparation methods and application thereof
CN105576204B (en) * 2015-12-23 2018-10-09 厦门大学 A kind of compound carbon coating cobalt phosphate lithium material of graphene and the preparation method and application thereof

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