CN105226272A - Lithium manganese phosphate-carbon composite and preparation method thereof, positive electrode and positive pole - Google Patents
Lithium manganese phosphate-carbon composite and preparation method thereof, positive electrode and positive pole Download PDFInfo
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- CN105226272A CN105226272A CN201410228553.2A CN201410228553A CN105226272A CN 105226272 A CN105226272 A CN 105226272A CN 201410228553 A CN201410228553 A CN 201410228553A CN 105226272 A CN105226272 A CN 105226272A
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- lithium
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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
Abstract
This application discloses a kind of preparation method of lithium manganese phosphate-carbon composite, comprising: step a), by the P source compound of carbon containing, Li source compound, manganese source compound and the mixing of doping metals source, obtains precursors; Step b), under protective atmosphere, is heat-treated precursors, obtains lithium manganese phosphate-carbon composite.Carbon-containing group in organic phosphorus sources in the present invention decomposes in heat treatment process, more uniform in-stiu coating layer is formed on lithium manganese phosphate primary particle surface, without the need to adding independent carbon source, the carbon coating layer on lithium manganese phosphate surface can be formed, and in-situ carbon coating layer can limit growing up of particle, make the size of primary particle in composite material less.
Description
Technical field
The application belongs to field of lithium ion battery material, particularly relates to a kind of lithium manganese phosphate-carbon composite and preparation method thereof, positive electrode and positive pole.
Background technology
There is the LiFePO of olivine structural
4material is used as anode material for lithium-ion batteries, and its theoretical capacity, at about 170mAh/g, has between Stability Analysis of Structures and electrolyte the plurality of advantages such as reactivity is little, fail safe is high, circulating battery is good simultaneously, achieved large-scale production and sale.But, LiFePO
4material is lower due to removal lithium embedded potential plateau (about 3.4V), reduces cell integrated energy density.And LiMnPO
4be 4.1V to the operating voltage of Li, can at LiFePO
4basis on the energy density of raising about 20%, likely become the first-selection of the positive electrode of following batteries of electric automobile.
Restriction LiMnPO
4the main cause of large-scale application is that it compares LiFePO
4worse electronic conductivity (<10
10scm
1) and lithium ion diffusion rate, cause charge/discharge capacity extremely low, battery high rate performance is poor.And in order to improve lithium ion transport efficiency and electrical conductivity efficiency, lithium manganese phosphate particle must be carried out nanometer and material with carbon-coated surface simultaneously.Although there is report to adopt the method such as hydro-thermal, collosol and gel to obtain nanoscale lithium manganese phosphate material, preparation method is complicated.
The high temperature solid-phase sintering method that suitability for industrialized production adopts can only obtain the lithium manganese phosphate particle of micron or submicron-scale usually.In addition, undersized lithium manganese phosphate particle can be reunited and be formed larger second particle in sintering process, causes the lithium manganese phosphate primary particle material with carbon-coated surface being in second particle inside imperfect.Even if add the carbon source of more in presoma, also can only form very thick coating layer on second particle surface, lithium ion and the electronic transmission performance of material monolithic can not be improved.
Summary of the invention
The object of the invention is to for deficiency of the prior art, a kind of lithium manganese phosphate-carbon composite and preparation method thereof, positive electrode and positive pole are provided.
For achieving the above object, the invention provides following technical scheme:
This application discloses a kind of lithium manganese phosphate-carbon composite, comprising general formula is LiMn
xm
1-xpO
4lithium manganese phosphate and carbon, wherein, 0.6≤x≤1, M be selected from Fe, Co, Ni, Mg, Cu, Zn, Zr, Ti, Al, Cr, Ge one or more.
Preferably, in above-mentioned lithium manganese phosphate-carbon composite, the content of described carbon is 1wt%-15wt%.
Correspondingly, disclosed herein as well is a kind of preparation method of lithium manganese phosphate-carbon composite, comprising:
Step a), by the P source compound of carbon containing, Li source compound, manganese source compound and the mixing of doping metals source, obtains precursors;
Step b), under protective atmosphere, is heat-treated precursors, obtains lithium manganese phosphate-carbon composite.
4, the preparation method of lithium manganese phosphate-carbon composite according to claim 3, is characterized in that: in described step b, and the heat treated temperature of described precursors is 400 DEG C ~ 900 DEG C, and the heat treated time is 1 ~ 48 hour.
Preferably, in the preparation method of above-mentioned lithium manganese phosphate-carbon composite, the P source compound of described carbon containing is selected from but is not limited to ammonium alcohol polyvinyl phosphate, ethylenediamine-phosphoric acid composite, propane diamine-phosphoric acid composite, tributyl phosphate, triethyl phosphate or ethylenediamine tetramethylene phosphoric acid.
Preferably, in the preparation method of above-mentioned lithium manganese phosphate-carbon composite, described Li source compound is selected from lithium hydroxide, lithium carbonate, lithium chloride, lithium acetate, lithium sulfate, lithium nitrate, lithium iodide, tert-butyl alcohol lithium, lithium benzoate, lithium formate, lithium fluoride, lithium chromate, four water citric acid lithiums, tetrachloro-lithium aluminate, lithium bromide, LiBF4, lithium phosphate, phosphoric acid hydrogen two lithium, lithium dihydrogen phosphate or lithium oxalate.
Preferably, in the preparation method of above-mentioned lithium manganese phosphate-carbon composite, described manganese source compound is selected from mangano-manganic oxide, manganese sesquioxide managnic oxide, manganese carbonate, manganese dioxide, manganous hydroxide, manganese acetate, four water manganese acetates, manganous chloride, four water manganous chloride, manganese tetrachloride, manganese sulfate, manganese sulfate monohydrate, sulfate dihydrate manganese, three water manganese sulfates, four water manganese sulfates, Manganese sulfate pentahydrate, six water manganese sulfates, seven water manganese sulfate or manganese nitrates.
Preferably, in the preparation method of above-mentioned lithium manganese phosphate-carbon composite, in described doping metals source, anion is not specifically limited, and such as can use sulfate, nitrate, hydrochloride, acetate, oxalates, phosphate etc.Viewed from the angle avoiding residual impurity obtained positive electrode active materials, preferably use acylate, as acetate or sulfate etc.Such as can be selected from but be not limited in the soluble metal compound of Fe, Co, Ni, Mg, Cu, Zn, Zr, Ti, Al, Cr, Ni, Ge etc. one or more combination, further it can be selected from but be not limited to ferric phosphate, ferrous oxalate, magnesium oxalate, magnesium acetate, ferrous sulfate, cobalt acetate, copper sulphate, nickel acetate, nickelous sulfate, magnesium acetate, zinc acetate or ferric nitrate.
Preferably; in the preparation method of above-mentioned lithium manganese phosphate-carbon composite; described protective atmosphere is the confining gas environment with corrosion protection component; in order to stop any component in specific reaction system and allogenic material react or import allogenic material in specific reaction system, one or more mist of the preferred free nitrogen of described protective atmosphere, argon gas, argon hydrogen gaseous mixture, nitrogen and hydrogen mixture.
The application also discloses a kind of positive electrode of secondary cell, and comprising general formula is LiMn
xm
1-xpO
4lithium manganese phosphate and carbon, wherein, 0.6≤x≤1, M be selected from Fe, Co, Ni, Mg, Cu, Zn, Zr, Ti, Al, Cr, Ge one or more.
Disclosed herein as well is a kind of anode of secondary battery, comprise matrix and the coating material being placed in matrix surface, described coating material comprises: above-mentioned positive electrode, electric conducting material and bonding agent.
Compared with prior art, the invention has the advantages that:
(1) carbon-containing group in organic phosphorus sources decomposes in heat treatment process, forms more uniform in-stiu coating layer on lithium manganese phosphate primary particle surface;
(2) without the need to adding independent carbon source, the carbon coating layer on lithium manganese phosphate surface can be formed;
(3) in-situ carbon coating layer can limit growing up of particle, makes the size of primary particle in composite material less.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present application or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, the accompanying drawing that the following describes is only some embodiments recorded in the application, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Figure 1 shows that scanning electron microscopy (SEM) photo of lithium manganese phosphate-carbon composite in the specific embodiment of the invention 1;
Figure 2 shows that transmission electron microscope (TEM) photo of lithium manganese phosphate-carbon composite in the specific embodiment of the invention 1;
Figure 3 shows that X-ray diffraction spectrum (XRD) collection of illustrative plates of lithium manganese phosphate-carbon composite in the specific embodiment of the invention 1.
Embodiment
For making the object, technical solutions and advantages of the present invention clearly, below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in detail.The example of these preferred implementations illustrates in the accompanying drawings.Shown in accompanying drawing and the embodiments of the present invention described with reference to the accompanying drawings be only exemplary, and the present invention is not limited to these execution modes.
At this, also it should be noted that, in order to avoid the present invention fuzzy because of unnecessary details, illustrate only in the accompanying drawings with according to the closely-related structure of the solution of the present invention and/or treatment step, and eliminate other details little with relation of the present invention.
embodiment 1
Phosphoric acid-ethylenediamine compound, manganese acetate, lithium carbonate and 10mL ethanol ball milling 6 hours are taken according to the ratio of Li/Mn/P elemental mole ratios 1:1:1, take out after drying, in blanket of nitrogen, 600 DEG C of heat treatment 12h obtain lithium manganese phosphate-carbon composite, and it mainly comprises general formula is LiMnPO
4compound and 3% carbon.
Fig. 1 is the SEM photo of the lithium manganese phosphate-carbon composite of preparation in embodiment 1, and the primary particle size of visible material is about 50nm.
Fig. 2 is the TEM photo of lithium manganese phosphate-carbon composite of preparation in embodiment 1, and visible particle Surface coating is had an appointment the thick amorphous carbon of 2nm.
Fig. 3 is the XRD collection of illustrative plates of the lithium manganese phosphate-carbon composite of preparation in embodiment 1, and visible sample is the lithium manganese phosphate of pure phase, without obvious dephasign.
embodiment 2
Mix according to the ratio weighing polyvinyl alcohol ammonium phosphate of Li/Mn/Fe/P elemental mole ratios 1:0.8:0.2:1, manganese acetate, ferrous oxalate, lithium carbonate and 10mL ethanol, in argon gas atmosphere, 700 DEG C of heat treatment 10h obtain lithium manganese phosphate-carbon composite, and it mainly comprises general formula is LiMn
0.8fe
0.2pO
4compound and 1% carbon, primary particle is about 60nm.
embodiment 3
Triethyl phosphate, manganese acetate, nickel acetate, lithium carbonate and 10mL ethanol ball milling 12 hours are taken according to the ratio of Li/Mn/Ni/P elemental mole ratios 1:0.9:0.1:1, take out after drying, in argon hydrogen (5% hydrogen) atmosphere, 600 DEG C of heat treatment 12h obtain lithium manganese phosphate-carbon composite, and it mainly comprises general formula is LiMn
0.9ni
0.1pO
4compound and 4% carbon, primary particle is about 60nm.
embodiment 4
Tributyl phosphate, manganese acetate, ferrous oxalate, magnesium oxalate, lithium carbonate and 10mL ethanol ball milling 6 hours are taken according to the ratio of Li/Mn/Fe/Mg/P elemental mole ratios 1:0.8:0.1:0.1:1, take out after drying, in blanket of nitrogen, 800 DEG C of heat treatment 12h obtain lithium manganese phosphate-carbon composite, and it mainly comprises general formula is LiMn
0.8fe
0.1mg
0.1pO
4compound and 3% carbon, primary particle is about 100nm.
embodiment 5
Ethylenediamine tetramethylene phosphoric acid, manganese carbonate, lithium hydroxide and 10mL ethanol ball milling 6 hours are taken according to the ratio of Li/Mn/P elemental mole ratios 1:1:1, take out after drying, in blanket of nitrogen, 600 DEG C of heat treatment 12h obtain lithium manganese phosphate-carbon composite, and it mainly comprises general formula is LiMnPO
4compound and 5% carbon, primary particle is about 70nm.
In sum, preparation method of the present invention is simple, and be easy to realize large-scale production, the composite material of preparation can be applicable to lithium rechargeable battery, has higher specific capacity.
Finally, also it should be noted that, term " comprises ", " comprising " or its any other variant are intended to contain comprising of nonexcludability, thus make to comprise the process of a series of key element, method, article or equipment and not only comprise those key elements, but also comprise other key elements clearly do not listed, or also comprise by the intrinsic key element of this process, method, article or equipment.
Claims (10)
1. lithium manganese phosphate-carbon composite, is characterized in that, comprising general formula is LiMn
xm
1-xpO
4lithium manganese phosphate and carbon, wherein, 0.6≤x≤1, M be selected from Fe, Co, Ni, Mg, Cu, Zn, Zr, Ti, Al, Cr, Ge one or more.
2. lithium manganese phosphate-carbon composite according to claim 1, is characterized in that: the content of described carbon is 1wt%-15wt%.
3. the preparation method of the lithium manganese phosphate-carbon composite described in claim 1 or 2, is characterized in that, comprising:
Step a), by the P source compound of carbon containing, Li source compound, manganese source compound and the mixing of doping metals source, obtains precursors;
Step b), under protective atmosphere, is heat-treated precursors, obtains lithium manganese phosphate-carbon composite.
4. the preparation method of lithium manganese phosphate-carbon composite according to claim 3, is characterized in that: in described step b, and the heat treated temperature of described precursors is 400 DEG C ~ 900 DEG C, and the heat treated time is 1 ~ 48 hour.
5. the preparation method of lithium manganese phosphate-carbon composite according to claim 3, is characterized in that: the P source compound of described carbon containing is selected from but is not limited to ammonium alcohol polyvinyl phosphate, ethylenediamine-phosphoric acid composite, propane diamine-phosphoric acid composite, tributyl phosphate, triethyl phosphate or ethylenediamine tetramethylene phosphoric acid.
6. the preparation method of lithium manganese phosphate-carbon composite according to claim 3, is characterized in that: described Li source compound is selected from lithium hydroxide, lithium carbonate, lithium chloride, lithium acetate, lithium sulfate, lithium nitrate, lithium iodide, tert-butyl alcohol lithium, lithium benzoate, lithium formate, lithium fluoride, lithium chromate, four water citric acid lithiums, tetrachloro-lithium aluminate, lithium bromide, LiBF4, lithium phosphate, phosphoric acid hydrogen two lithium, lithium dihydrogen phosphate or lithium oxalate.
7. the preparation method of lithium manganese phosphate-carbon composite according to claim 3, is characterized in that: described manganese source compound is selected from mangano-manganic oxide, manganese sesquioxide managnic oxide, manganese carbonate, manganese dioxide, manganous hydroxide, manganese acetate, four water manganese acetates, manganous chloride, four water manganous chloride, manganese tetrachloride, manganese sulfate, manganese sulfate monohydrate, sulfate dihydrate manganese, three water manganese sulfates, four water manganese sulfates, Manganese sulfate pentahydrate, six water manganese sulfates, seven water manganese sulfate or manganese nitrates.
8. the preparation method of lithium manganese phosphate-carbon composite according to claim 3, is characterized in that: described doping metals source is one or more the combination in Fe, Co, Ni, Mg, Cu, Zn, Zr, Ti, Al, Cr, Ge metallic compound.
9. a positive electrode for secondary cell, is characterized in that, comprising general formula is LiMn
xm
1-xpO
4lithium manganese phosphate and carbon, wherein, 0.6≤x≤1, M be selected from Fe, Co, Ni, Mg, Cu, Zn, Zr, Ti, Al, Cr, Ge one or more.
10. an anode of secondary battery, is characterized in that, comprise matrix and the coating material being placed in matrix surface, described coating material comprises: positive electrode according to claim 9, electric conducting material and bonding agent.
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Cited By (3)
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| CN109119615A (en) * | 2018-08-28 | 2019-01-01 | 重庆大学 | A kind of lithium manganese phosphate composite positive pole and preparation method thereof that doped metallic elements are modified |
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