CN103000879A - Preparation method of spinel type lithium-nickel-manganese oxide with one-dimensional porous structure - Google Patents
Preparation method of spinel type lithium-nickel-manganese oxide with one-dimensional porous structure Download PDFInfo
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Abstract
The invention relates to a preparation method of a spinel type lithium-nickel-manganese oxide with a one-dimensional porous structure, which comprises the following steps of: mixing a manganese salt solution with an oxalic acid or ammonium oxalate solution, and stirring for reaction; separating, depositing, and drying to obtain a manganous oxalate micron rod with a one-dimensional structure; and roasting the manganous oxalate micron rod at high temperature in the presence of air or oxygen, then uniformly mixing with a lithium source and a nickel source, and finally roasting the obtained mixture at high temperature to prepare the spinel type lithium-nickel-manganese oxide with the one-dimensional porous structure. The spinel type lithium-nickel-manganese oxide with the one-dimensional porous structure, which is disclosed by the invention, shows the excellent high-current discharge property due to less inside granule composition and larger specific area, enhances the endurance degree of a material on the volume change of the process of taking off or embedding lithium through the inside unique microstructure, effectively enhances the cycling stability of the material and is an ideal electrode material; and the preparation method disclosed by the invention is simple in process, easy to implement and conductive to popularization and application.
Description
Technical field
The present invention relates to the preparation of anode active material of lithium ion battery, particularly a kind of preparation method with spinel-type Li-Ni-Mn-O of one dimension loose structure.
Background technology
Lithium ion battery have operating voltage height, energy density large, have extended cycle life, operating temperature range is wide and the advantage such as safe memory-less effect, being the power supply that most consumption electronic products adopt, also is a kind of very promising used for electric vehicle electrical source of power simultaneously.Lithium ion battery mainly is comprised of positive pole, negative pole, barrier film and electrolyte four parts, and positive pole is one of key factor that determines performance of lithium ion battery usually.The positive electrode that current business-like lithium ion battery adopts is cobalt acid lithium, but its price, environment and safety problem have limited its application in electrokinetic cell.Therefore cheap, the environmental friendliness of development cost and safe and reliable substitution material become the main target of anode material for lithium-ion batteries development.LiMn2O4 has spinel structure, its good stability, price are low, environment-protecting asepsis and good heavy current, it is a kind of positive electrode that application prospect is arranged very much, referring to O.K.Park, Y.Cho, S.Lee, et al.Who will drive electric vehicles, olivine or spinel Energy Environ.Sci., 2011,4:1621.The spinel-type Li-Ni-Mn-O is that the part manganese in the LiMn2O4 is replaced with nickel, its structure and LiMn2O4 are similar, have good stability and good heavy-current discharge performance, its voltage platform exceeds about 0.7V than LiMn2O4 simultaneously, therefore its power density and energy density are higher than LiMn2O4, also are a kind of positive electrodes that using value is arranged, referring to J.B.Goodenough and Y.Kim.Challenges for Rechargeable Li Batteries.Chem.Mater., 2009,22:587.
At present, the subject matter that faces in commercial applications of LiMn2O4 is the decline of its capacity in charge and discharge process.Manganese in the LiMn2O4 is with Mn
3+And Mn
4+Form exists, wherein Mn
3+Change in volume and the phase transformation in the removal lithium embedded process that disproportionation is decomposed, the Jahn-Teller effect causes be the main cause that causes its inducing capacity fading, referring to L.Xiong, Y.Xu, and T.Tao.Excellent stability of spinel LiMn2O4-basedcomposites for lithium ion batteries.J.Mater.Chem., 2012, DOI:10.1039/c2jm34717b.In Li-Ni-Mn-O, nearly all manganese is all with Mn
4+Form exists, and has at utmost reduced Mn
3+Disproportionation decompose and the Jahn-Teller effect, but its capacity still has obvious decline in charge and discharge process, this may be to be caused by the phase transformation in the side reaction of electrolyte and the removal lithium embedded process.In addition, in order to satisfy electrokinetic cell to the harsh requirement of positive electrode heavy-current discharge performance, the multiplying power discharging property of this bi-material is still waiting further reinforcement.Therefore, structure and the pattern by designing material is very important to improve its cyclical stability and to strengthen its multiplying power discharging property.
Have the electrode material of one dimension micro-nano structure because owing to comprise effective one dimension electric transmission path and short ion the evolving path, and show superior chemical property.Electrode material with loose structure then can cushion structural strain in the charge and discharge process, and loose structure can improve the contact area of active material and electrolyte, thereby presents good cycle performance and high rate performance.Prediction has the advantage that a peacekeeping porous micro-nano structure material probably has these two kinds of structures simultaneously simultaneously thus, and its unique internal microstructure can be brought outstanding chemical property.
Summary of the invention
The object of the invention is to for the problems referred to above, a kind of preparation method with spinel-type Li-Ni-Mn-O of one dimension loose structure is proposed, the method is to be precursor with manganese oxalate, the solid phase insertion reaction that keeps by pattern prepares the spinel-type Li-Ni-Mn-O with one dimension loose structure, gained spinel-type Li-Ni-Mn-O shows good cyclical stability and excellent heavy-current discharge performance as anode material of lithium battery.
Technical scheme of the present invention:
A kind of preparation method with spinel-type Li-Ni-Mn-O of one dimension loose structure, step is as follows:
1) preparation of the manganese oxalate micron bar of one-dimentional structure
Manganese salt solution is mixed with oxalic acid or ammonium oxalate solution and stirring reaction 20 minutes, and precipitation and separation is also dry, namely obtains the manganese oxalate micron bar of one-dimentional structure, and its diameter is that 0.2-3 μ m, fineness ratio are 1:2-100;
2) preparation of spinel-type Li-Ni-Mn-O
With above-mentioned manganese oxalate micron bar with one-dimentional structure in the presence of air or oxygen at 300-600 ℃ of roasting 2-15 hour, then mix with lithium source and nickel source, at last with the gained mixture under the air or oxygen atmosphere 300-900 ℃ roasting 6-34 hour, preparation spinel-type Li-Ni-Mn-O, it has the one dimension loose structure, diameter is that 0.2-3 μ m, fineness ratio are that 1:2-20, average pore size are 10-20nm, and specific area is 4-7m
2/ g.
Described manganese salt is manganese chloride, manganese sulfate, manganese nitrate or manganese acetate, and the concentration of manganese salt solution is the 0.05-1.5 mol/L; The concentration of oxalic acid or ammonium oxalate solution is the 0.05-1.5 mol/L; Manganese salt solution and oxalic acid or ammonium oxalate solution volume ratio are 1:1-8.
Described lithium source is lithium hydroxide, lithium nitrate or lithium acetate, and the nickel source is nickel acetate, nickel nitrate, nickel chloride or nickelous sulfate, and the lithium in the manganese in the manganese oxalate micron bar, the lithium source and the mol ratio of the nickel in the nickel source are 1.5:1-1.05:0.5.
A kind of described application with spinel-type Li-Ni-Mn-O of one dimension loose structure, for the preparation of lithium battery anode, described lithium battery comprises positive pole, lithium anode, barrier film and electrolyte, anodal by electrode material, conductive agent and binding agent form, wherein electrode material comprises one dimension porous spinelle type Li-Ni-Mn-O, conductive agent is carbon nano-fiber, electrically conductive graphite, acetylene black, the mixture of one or more arbitrary proportions among the Super P, binding agent is polytetrafluoroethylene or Kynoar, the mass percent of conductive agent and binding agent is respectively 20%-5%, 10%-5%, spinel-type Li-Ni-Mn-O are surplus; Described barrier film is three layers of barrier film that polyethylene or polypropylene consist of; Described electrolyte is the mixture of one or more arbitrary proportions of ethyl carbonate (EC), propene carbonate (PC), dimethyl carbonate (DMC), diethyl carbonate (DEC).
Advantage of the present invention is: have the spinel-type Li-Ni-Mn-O of one dimension loose structure owing to have less internal particle composition and larger specific area, make it show excellent heavy-current discharge performance, and its inner unique microstructure has improved material the change in volume in the removal lithium embedded process has been restrained oneself degree, Effective Raise the cyclical stability of material, be a kind of desirable electrode material; This preparation method's technique is simple, easy to implement, is conducive to apply.
Description of drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of manganese oxalate micron bar.
Fig. 2 is the scanning electron microscope (SEM) photograph of spinel-type Li-Ni-Mn-O multi-pore micron rod.
Fig. 3 is the charging and discharging curve of the circulation second time take spinel-type Li-Ni-Mn-O multi-pore micron rod as anodal lithium battery.
Fig. 4 is take the cyclical stability figure of spinel-type Li-Ni-Mn-O multi-pore micron rod as anodal lithium battery.
Specific embodiment
Embodiment:
A kind of preparation method with spinel-type Li-Ni-Mn-O of one dimension loose structure, step is as follows:
1) preparation of the manganese oxalate micron bar of one-dimentional structure
The 20mL 0.4M manganese chloride aqueous solution is mixed with 20mL 0.4M oxalic acid aqueous solution and stirred 20 minutes, precipitation and separation is also dry, namely obtain the manganese oxalate micron bar of one-dimentional structure, Fig. 1 is the scanning electron microscope (SEM) photograph of manganese oxalate micron bar, shows among the figure that the diameter of this manganese oxalate micron bar is 1-3 μ m.
2) preparation of spinel-type Li-Ni-Mn-O
The manganese oxalate micron bar that above-mentioned 500mg is had an one-dimentional structure in air atmosphere 500 ℃ of roastings 10 hours, then mix with 181mg two hydration lithium acetates and 210mg four hydration nickel acetates, with the 700 ℃ of roastings 10 hours under the air or oxygen atmosphere of gained mixture, preparation spinel-type Li-Ni-Mn-O, Fig. 2 is the scanning electron microscope (SEM) photograph of spinel-type Li-Ni-Mn-O multi-pore micron rod, the diameter that shows this multi-pore micron rod among the figure is 1-3 μ m, and length is 10-20 μ m.
With the excellent application as high-performance button-type lithium cell positive pole of spinel-type Li-Ni-Mn-O multi-pore micron of above-mentioned preparation, step is as follows:
1) preparation of Li-Ni-Mn-O positive pole
75wt% porous spinelle type Li-Ni-Mn-O, 20wt% acetylene black and 5wt% Kynoar are added the even pulpous state of 1-METHYLPYRROLIDONE furnishing, be coated in thickness and be 500 μ m, diameter and be on the aluminium foil disk of 12mm as pole piece, pole piece was 100 ℃ of vacuumizes 12 hours, then press down 1 minute at 20MPa pressure, obtain spinel-type Li-Ni-Mn-O positive plate, wherein the quality of spinel-type Li-Ni-Mn-O is 1mg;
2) button cell assembling
Be that the lithium sheet of 2mm is cuted off the feet into the disk of diameter 14mm as negative plate with thickness, barrier film is the Celgard 2320 that polyethylene/polypropylene/polyethylene trilamellar membrane forms, electrolyte is the ethyl carbonate (EC)/dimethyl carbonate (DMC) solution of concentration 1.0mol/L lithium hexafluoro phosphate (LiPF6), and the volume ratio of EC and DMC is 1:1.Above-mentioned positive and negative plate, barrier film and electrolyte are assembled into CR2032 button lithium battery in being full of the glove box of argon gas.
This button lithium battery performance test:
Fig. 3 is the charging and discharging curve of the circulation second time take spinel-type Li-Ni-Mn-O multi-pore micron rod as anodal lithium battery, and its discharge capacity reaches 133mAh g
-1Fig. 4 is take the cyclical stability figure of spinel-type Li-Ni-Mn-O multi-pore micron rod as anodal lithium battery, shows among the figure: after 200 circulations, Capacitance reserve is at 105mAhg
-1, capability retention reaches 79%.
Claims (4)
1. preparation method with spinel-type Li-Ni-Mn-O of one dimension loose structure is characterized in that step is as follows:
1) preparation of the manganese oxalate micron bar of one-dimentional structure
Manganese salt solution is mixed with oxalic acid or ammonium oxalate solution and stirring reaction 20 minutes, and precipitation and separation is also dry, namely obtains the manganese oxalate micron bar of one-dimentional structure, and its diameter is that 0.2-3 μ m, fineness ratio are 1:2-100;
2) preparation of spinel-type Li-Ni-Mn-O
With above-mentioned manganese oxalate micron bar with one-dimentional structure in the presence of air or oxygen at 300-600 ℃ of roasting 2-15 hour, then mix with lithium source and nickel source, at last with the gained mixture under the air or oxygen atmosphere 300-900 ℃ roasting 6-34 hour, preparation spinel-type Li-Ni-Mn-O, it has the one dimension loose structure, diameter is that 0.2-3 μ m, fineness ratio are that 1:2-20, average pore size are 10-20nm, and specific area is 4-7m2/g.
2. the described preparation method that the spinel-type Li-Ni-Mn-O of one dimension loose structure is arranged according to claim 1, it is characterized in that: described manganese salt is manganese chloride, manganese sulfate, manganese nitrate or manganese acetate, the concentration of manganese salt solution is the 0.05-1.5 mol/L; The concentration of oxalic acid or ammonium oxalate solution is the 0.05-1.5 mol/L; Manganese salt solution and oxalic acid or ammonium oxalate solution volume ratio are 1:1-8.
3. the described preparation method that the spinel-type Li-Ni-Mn-O of one dimension loose structure is arranged according to claim 1, it is characterized in that: described lithium source is lithium hydroxide, lithium nitrate or lithium acetate, the nickel source is nickel acetate, nickel nitrate, nickel chloride or nickelous sulfate, and the lithium in the manganese in the manganese oxalate micron bar, the lithium source and the mol ratio of the nickel in the nickel source are 1.5:1-1.05:0.5.
4. application such as the prepared spinel-type Li-Ni-Mn-O with one dimension loose structure of claim, it is characterized in that: for the preparation of lithium battery anode, described lithium battery comprises positive pole, lithium anode, barrier film and electrolyte, anodal by electrode material, conductive agent and binding agent form, wherein electrode material comprises one dimension porous spinelle type Li-Ni-Mn-O, conductive agent is carbon nano-fiber, electrically conductive graphite, acetylene black, the mixture of one or more arbitrary proportions among the Super P, binding agent is polytetrafluoroethylene or Kynoar, the mass percent of conductive agent and binding agent is respectively 20%-5%, 10%-5%, spinel-type Li-Ni-Mn-O are surplus; Described barrier film is three layers of barrier film that polyethylene or polypropylene consist of; Described electrolyte is the mixture of one or more arbitrary proportions of ethyl carbonate (EC), propene carbonate (PC), dimethyl carbonate (DMC), diethyl carbonate (DEC).
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Cited By (7)
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| CN103367739A (en) * | 2013-07-18 | 2013-10-23 | 桂林电子科技大学 | Ellipsoidal porous-structured lithium manganate or nickel lithium manganate positive electrode material and preparation method thereof |
| CN103943848A (en) * | 2014-04-23 | 2014-07-23 | 合肥工业大学 | Preparation method of positive pole material of cobalt-based lithium ion battery with porous rod-like structure |
| CN104282889A (en) * | 2014-09-11 | 2015-01-14 | 浙江南都电源动力股份有限公司 | Preparation method of manganese oxalate feed liquor and spinel lithium manganate |
| CN105609753A (en) * | 2015-12-14 | 2016-05-25 | 青岛大学 | Preparation method for one-dimensional multi-layer porous fibrous positive electrode material of lithium ion battery |
| CN111924882A (en) * | 2020-07-03 | 2020-11-13 | 山东科源新材料有限公司 | Porous lithium manganate positive electrode material and preparation method thereof |
| CN112811882A (en) * | 2021-01-11 | 2021-05-18 | 湖南省美程陶瓷科技有限公司 | High-stability sensor ceramic material and preparation method thereof |
| US11111576B2 (en) | 2015-06-10 | 2021-09-07 | Forschungszentrum Juelich Gmbh | Method for producing nanostructured layers |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103367739A (en) * | 2013-07-18 | 2013-10-23 | 桂林电子科技大学 | Ellipsoidal porous-structured lithium manganate or nickel lithium manganate positive electrode material and preparation method thereof |
| CN103943848A (en) * | 2014-04-23 | 2014-07-23 | 合肥工业大学 | Preparation method of positive pole material of cobalt-based lithium ion battery with porous rod-like structure |
| CN104282889A (en) * | 2014-09-11 | 2015-01-14 | 浙江南都电源动力股份有限公司 | Preparation method of manganese oxalate feed liquor and spinel lithium manganate |
| CN104282889B (en) * | 2014-09-11 | 2017-05-03 | 浙江南都电源动力股份有限公司 | Preparation method of manganese oxalate feed liquor and spinel lithium manganate |
| US11111576B2 (en) | 2015-06-10 | 2021-09-07 | Forschungszentrum Juelich Gmbh | Method for producing nanostructured layers |
| CN105609753A (en) * | 2015-12-14 | 2016-05-25 | 青岛大学 | Preparation method for one-dimensional multi-layer porous fibrous positive electrode material of lithium ion battery |
| CN105609753B (en) * | 2015-12-14 | 2019-04-30 | 青岛大学 | The preparation method of one-dimensional multi-layer porous fibrous anode material for lithium-ion batteries |
| CN111924882A (en) * | 2020-07-03 | 2020-11-13 | 山东科源新材料有限公司 | Porous lithium manganate positive electrode material and preparation method thereof |
| CN112811882A (en) * | 2021-01-11 | 2021-05-18 | 湖南省美程陶瓷科技有限公司 | High-stability sensor ceramic material and preparation method thereof |
| CN112811882B (en) * | 2021-01-11 | 2022-04-22 | 湖南省美程陶瓷科技有限公司 | High-stability sensor ceramic material and preparation method thereof |
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