CN104037411A - Multielement doped lithium phosphate anode material and preparation method - Google Patents

Multielement doped lithium phosphate anode material and preparation method Download PDF

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Publication number
CN104037411A
CN104037411A CN201410208969.8A CN201410208969A CN104037411A CN 104037411 A CN104037411 A CN 104037411A CN 201410208969 A CN201410208969 A CN 201410208969A CN 104037411 A CN104037411 A CN 104037411A
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source compound
anode material
lithium phosphate
lithium
preparation
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肖文杰
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SHENZHEN SJY ENERGY TECHNOLOGY Co Ltd
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SHENZHEN SJY ENERGY TECHNOLOGY Co Ltd
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    • 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
    • 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
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • 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
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • 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

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Composite Materials (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention aims at providing a multielement doped lithium phosphate anode material which is good in conductivity and long in cycle life, and improves the energy density of an anode material for the existing power cell, and a preparation method of the anode material. According to the anode material and the preparation method, the conductivity and the cycle life of the lithium phosphate anode material are improved and prolonged successfully and/or the energy density of the anode material for the existing power cell is improved by selecting a doped element combination and strictly controlling the content of components of the combination. In a synthetic process of the anode material, little iron in lithium iron phosphate is substituted by doping metal ions (Ti<4+> and Mn<4+>) to improve the conductivity of a lithium iron phosphate material, and the conductivity of an LiFe1-x-yTi0.5xMn0.1-yPO4/C composite material is improved mainly by adopting a method of performing carbon coating on the lithium iron phosphate material twice by blending twice and adding a carbon source twice, so that the high multiplying power charge and discharge energy of the anode material is further improved. The anode material and the preparation method are applicable to the field of cells.

Description

A kind of multi-element doping lithium phosphate cathode material and preparation method
Technical field
The present invention relates to a kind of anode material for lithium ion battery and preparation method thereof, more particularly, the present invention relates to a kind of multi-element doping lithium phosphate cathode material and preparation method thereof.
Background technology
The LiFePO of olivine-type structure 4have environmentally friendly, energy density is high, excellent cycle performance especially, the remarkable advantages such as best security performance, and its synthesis material aboundresources, cheap, unanimously be known as is to manufacture high safety, low cost, the best positive electrode of long-life power lithium-ion battery, be one of new energy materials of tool potentiality, become the manufacturing object of pursuing of battery industry and new energy materials.But LiFePO4 exists the defect of material self character: conductance is low, and high rate performance is poor, this has limited its extensive use in practical field greatly; And preparation process relative complex (raw material type is many, difficult mixing); Synthesis condition is harsh (inert gas shielding) comparatively; To equipment requirement higher (will have good air-tightness), this has just further limited its large-scale industrialization.
Chinese patent CN101521276 discloses a kind of preparation method of lithium ion battery positive material coated with carbon: a certain amount of lithium ion battery positive material powder is put into polyacrylonitrile solution; fully stir and evenly mix; after heating evaporation solvent; under air atmosphere; put into baking oven and heat 2～4h at 150～300 DEG C; obtain black solid; again the black solid of gained is put into high temperature furnace; 400～1200 DEG C of heating 0.5～4h under inert gas shielding, just obtain surface and have been coated the lithium ion battery powdery positive electrode of carbon.
Chinese patent CN101521278 discloses a kind of anode composite material of lithium ion battery preparation method: adopt high-temperature decomposition to prepare δ-MnO 2; Adopt ion implantation to prepare composite material δ-MnO 2-X, wherein X is transition metal, by the δ-MnO making 2taking sheet as matrix, then implanting transition metal ion; Composite material is made to battery anode slice; Scrape δ-MnO that top layer forms 2-Xmake positive electrode active materials and mix in proportion with other material and make based lithium-ion battery positive plate through film, dry, compressing tablet, the step such as dry, weigh.Owing to adopting ion implantation technique, inject a certain amount of transition metal ions in the table of layered manganese oxide, make layered manganese oxide modification, strengthen lithium ion in the electrochemical intercalation of this material/deviate from ability, improve stratiform MnO 2specific discharge capacity, the lithium ion battery of making has advantages of that cost is low, performance good, environmental protection.But its preparation method complexity, needs professional and technical personnel to have operated, and cost of labor is higher.
Summary of the invention
Technical problem to be solved by this invention is to overcome the deficiencies in the prior art, provide a kind of and conduct electricity very well, have extended cycle life and improve existing electrokinetic cell positive electrode energy density multi-element doping lithium phosphate cathode material and prepare the method for this positive electrode.
The technical scheme that a kind of multi-element doping lithium phosphate cathode material of the present invention adopts is: this positive electrode general formula is LiFe 1-x-yti 0.5xMn 0.1-yPO 4/ C, with LiFe 1-x-yti 0.5xMn 0.1-yPO 4/ C is base material, base material is coated with material with carbon element particulate layer, base material and material with carbon element particulate layer are combined into composite particles, and composite particles is dispersed in the conductive network by material with carbon element ultrafine particles composition, wherein 0.03≤(x/2+y)≤0.10,0.02≤x≤y≤0.08, C is generated by organic carbon source compound decomposition.
Further, described organic carbon source compound is the one in glucose, sucrose, citric acid or polyethylene glycol.
Further, the addition of described organic carbon source compound is the 1-10% of base material raw material total weight.
Further, the particle diameter of described composite particles is between 0.5～5 μ m, and its specific area is 12-35 m 2/ g.
Further, the diameter of described material with carbon element particulate is between 5～50 nm.
The technical scheme that the preparation method of a kind of multi-element doping lithium phosphate cathode material of the present invention adopts is that the method comprises the following steps:
(1) by the manganese in the titanium in the iron in the lithium in Li source compound, Fe source compound, titanium source compound, manganese source compound, ammonium dihydrogen phosphate, according to 1 ﹕, (1-x-y) ﹕ 0.5x ﹕ (mix by the ratio of the mol ratio of 0.1-y) ﹕ 1, add carbon or organic carbon source compound simultaneously, the addition of carbon or organic carbon source compound is 1～10% of base material raw material total weight, form raw mixture, wherein, 0.03≤(x/2+y)≤0.10,0.02≤x≤y≤0.08;
(2) raw mixture is scattered in water or ethanol or acetone solvent, the mass ratio of raw material solid and solvent is 1:1.5～2.5, rotating speed ball milling with 200-1000 r/min in high energy ball mill disperses 15～25 hours, the suspension obtaining is sprayed by high-speed centrifugal spray dryer dry, prepare forerunner's dispersion;
(3) in argon gas atmosphere, the programming rate by forerunner's dispersion powder with 1～5 DEG C/min, heat treatment 8～30h in the temperature range of 650～750 DEG C, then naturally cools to below 100 DEG C;
(4) will sieve through step (3) primary sintered material after treatment, and add organic carbon source compound to carry out carbon for the second time and be coated, then add deionized water, dry after ball milling;
(5) by step (4) gained material in argon gas atmosphere, with the programming rate of 1～5 DEG C/min, in the temperature range of 600～800 DEG C, carry out sintering processes 12～16h, then naturally cool to below 100 DEG C;
(6) in agitator, carry out mechanical fusion treatment, the rotating speed of agitator is 500～800 r/min, and time 50～200min obtains multi-element doping lithium phosphate cathode material.
Further, in described step (4), add the amount of deionized water to can be 30%～40% of primary sintered material; The ball material mass ratio of described ball milling can be (4～8): 1, and the time of described ball milling can be 3～5h, adopts spraying to be dried.
Further, in described step (2), it is 180～250 DEG C that described high-speed centrifugal spray dryer carries out spray-dired inlet temperature, and outlet temperature is 50～80 DEG C, and feeding speed is: 20～100 ml/min.
Further, described Li source compound is the one in lithium hydroxide, lithium carbonate, lithium acetate, lithium chloride, lithium nitrate, lithium oxalate; Described Fe source compound is the one in frerrous chloride, iron chloride, ironic citrate, iron hydroxide, ferrous lactate, ferric nitrate, ferrous oxide, ferrous oxalate; Described titanium source compound is the one of metatitanic acid, titanium trichloride, titanium tetrachloride, metatitanic acid; Described manganese source compound is the one in manganese chloride, manganous hydroxide, manganese carbonate, manganese nitrate, manganese dioxide.
The invention has the beneficial effects as follows: the present invention is in building-up process, except passing through doped metal ion (Ti 4+and Mn 4+), replace iron a small amount of in LiFePO4 to improve outside the conductivity of LiFePO 4 material, most importantly adopt by twice batching, add different carbon sources for twice, especially for the second time batching adds macromolecule organic carbon source, to the coated method of twice carbon of LiFePO 4 material, improves LiFe 1-x-yti 0.5xMn 0.1-yPO 4the conductivity of/C composite material; Further improve its greatly doubly forthright energy that discharges and recharges.Through facts have proved, the preparation method of this material is feasible, and effect is remarkable: the LiFe that adopts preparation method of the present invention to produce 1-x-yti 0.5xMn 0.1-yPO 4/ C composite material, tap density, at 0.8-1.3g/ml, is made after battery, and internal resistance is less than 30m Ω, and cycle performance excellence, and 800 weeks are unattenuated; Another large advantage of this invention is repeatedly coated sintering stable preparation process described in being exactly, and step is relatively simple, and particularly product reappearance is good, is very easy to realize industrialization and produces.
Brief description of the drawings
Fig. 1 is LiFe in the embodiment of the present invention 1 1-x-yti 0.5xMn 0.1-yPO 4the XRD figure of/C compound;
Fig. 2 is the LiFe making in the embodiment of the present invention 1 1-x-yti 0.5xMn 0.1-yPO 4the high rate performance result of/C compound during as anode material for lithium-ion batteries shows figure;
Fig. 3 is the LiFe that the embodiment of the present invention 1 makes 1-x-yti 0.5xMn 0.1-yPO 4/ C compound is as anode material for lithium-ion batteries, and the cycle performance result under C/2 multiplying power shows figure.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Prepare in accordance with the following methods positive electrode.
(1) by lithium hydroxide: frerrous chloride: titanium trichloride: manganese oxalate: ammonium dihydrogen phosphate mixes (x=y=0.02 wherein) according to the ratio of the mol ratio of 1:0.96:0.01: 0.08:1, add citric acid simultaneously, the addition of citric acid is 3% of base material raw material total weight (being the total weight of lithium source, source of iron, titanium source, titanium source, manganese source and ammonium dihydrogen phosphate), forms raw mixture;
(2) raw mixture is scattered in alcohol solvent, the mass ratio of solid and solvent is 1:1.5, rotating speed ball milling with 500 r/min in high energy ball mill disperses 20h, the suspension obtaining is sprayed dry by high-speed centrifugal spray dryer, spray-dired inlet temperature is 220 DEG C, outlet temperature is 50 DEG C, and feeding speed is: 50 ml/min prepare forerunner's dispersion;
(3), in argon gas atmosphere, forerunner's dispersion powder is warming up to 350 DEG C with the programming rate of 2 DEG C/min, constant temperature 3 hours; In argon gas atmosphere, be warming up to 720 DEG C with the programming rate of 2 DEG C/min, constant temperature 27 hours, then naturally cools to below 100 DEG C;
(4) primary sintered material after calcining is sieved, add glucose to carry out charcoal for the second time and be coated, then add deionized water, then add the amount of deionized water to can be 35% of primary sintered material, ball milling, the time of ball milling can be 4h, dry;
(5) by step (4) gained material in argon gas atmosphere, with the programming rate to 750 DEG C of 5 DEG C/min, then sintering 13h naturally cools to below 100 DEG C;
(6) after broken dispersion, carry out mechanical fusion treatment, rotating speed 500 r/min, time 50min, then sieves and obtains positive electrode.
The above-mentioned positive electrode preparing is tested and shown, the average diameter of composite particles is about 2.5 μ m, and the diameter of carbon granule is about 10 nm, and has formed the conductive network of continuous carbon, and specific area is 29.5 m 2/ g.
Fig. 1 shows the XRD collection of illustrative plates of this positive electrode, has shown to form the positive electrode of crystallization.
The above-mentioned positive electrode preparing is made after simulated battery according to method of the present invention, and charge-discharge test shows (discharge range is 2.0-4.5 V), as shown in Figure 2; And under the multiplying power condition of C/2, tested the cycle performance of battery, result is as shown in Figure 3.When test result shows phosphate cathode material of the present invention as lithium ion battery, there is extremely excellent cycle performance and discharge performance, and specific discharge capacity is high.
The present invention can be applicable to field of batteries.
It should be noted that, above-mentionedly only describe the present invention with preferred embodiment, can not limit to interest field of the present invention at this point, therefore in the situation that not departing from inventive concept, the equivalence that the content of all utilizations specification of the present invention and accompanying drawing part is carried out changes, and all reason is with being included within the scope of claim of the present invention.

Claims (9)

1. a multi-element doping lithium phosphate cathode material, is characterized in that: this material general formula is LiFe 1-x-yti 0.5xMn 0.1-yPO 4/ C, with LiFe 1-x-yti 0.5xMn 0.1-yPO 4/ C is base material, base material is coated with material with carbon element particulate layer, base material and material with carbon element particulate layer are combined into composite particles, and composite particles is dispersed in the conductive network by material with carbon element ultrafine particles composition, wherein 0.03≤(x/2+y)≤0.10,0.02≤x≤y≤0.08, C is generated by organic carbon source compound decomposition.
2. a kind of multi-element doping lithium phosphate cathode material according to claim 1, is characterized in that: described organic carbon source compound is the one in glucose, sucrose, citric acid or polyethylene glycol.
3. a kind of multi-element doping lithium phosphate cathode material according to claim 2, is characterized in that: the addition of described organic carbon source compound is the 1-10% of base material raw material total weight.
4. a kind of multi-element doping lithium phosphate cathode material according to claim 1, is characterized in that: the particle diameter of described composite particles is between 0.5～5 μ m, and its specific area is 12-35 m 2/ g.
5. a kind of multi-element doping lithium phosphate cathode material according to claim 1, is characterized in that: the diameter of described material with carbon element particulate is between 5～50 nm.
6. the preparation method of a kind of multi-element doping lithium phosphate cathode material as claimed in claim 1, is characterized in that, the method comprises the following steps:
(1) by the manganese in the titanium in the iron in the lithium in Li source compound, Fe source compound, titanium source compound, manganese source compound, ammonium dihydrogen phosphate, according to 1 ﹕, (1-x-y) ﹕ 0.5x ﹕ (mix by the ratio of the mol ratio of 0.1-y) ﹕ 1, add carbon or organic carbon source compound simultaneously, the addition of carbon or organic carbon source compound is 1～10% of base material raw material total weight, form raw mixture, wherein, 0.03≤(x/2+y)≤0.10,0.02≤x≤y≤0.08;
(2) raw mixture is scattered in water or ethanol or acetone solvent, the mass ratio of raw material solid and solvent is 1:1.5～2.5, rotating speed ball milling with 200-1000 r/min in high energy ball mill disperses 15～25 hours, the suspension obtaining is sprayed by high-speed centrifugal spray dryer dry, prepare forerunner's dispersion;
(3) in argon gas atmosphere, the programming rate by forerunner's dispersion powder with 1～5 DEG C/min, heat treatment 8～30h in the temperature range of 650～750 DEG C, then naturally cools to below 100 DEG C;
(4) will sieve through step (3) primary sintered material after treatment, and add organic carbon source compound to carry out carbon for the second time and be coated, then add deionized water, dry after ball milling;
(5) by step (4) gained material in argon gas atmosphere, with the programming rate of 1～5 DEG C/min, in the temperature range of 600～800 DEG C, carry out sintering processes 12～16h, then naturally cool to below 100 DEG C;
(6) in agitator, carry out mechanical fusion treatment, the rotating speed of agitator is 500～800 r/min, and time 50～200min obtains multi-element doping lithium phosphate cathode material.
7. the preparation method of a kind of multi-element doping lithium phosphate cathode material according to claim 6, is characterized in that: in described step (4), add the amount of deionized water to can be 30%～40% of primary sintered material; The ball material mass ratio of described ball milling can be (4～8): 1, and the time of described ball milling can be 3～5h, adopts spraying to be dried.
8. the preparation method of a kind of multi-element doping lithium phosphate cathode material according to claim 6, it is characterized in that: in described step (2), it is 180～250 DEG C that described high-speed centrifugal spray dryer carries out spray-dired inlet temperature, outlet temperature is 50～80 DEG C, and feeding speed is: 20～100 ml/min.
9. the preparation method of a kind of multi-element doping lithium phosphate cathode material according to claim 6, is characterized in that: described Li source compound is the one in lithium hydroxide, lithium carbonate, lithium acetate, lithium chloride, lithium nitrate, lithium oxalate; Described Fe source compound is the one in frerrous chloride, iron chloride, ironic citrate, iron hydroxide, ferrous lactate, ferric nitrate, ferrous oxide, ferrous oxalate; Described titanium source compound is the one of metatitanic acid, titanium trichloride, titanium tetrachloride, metatitanic acid; Described manganese source compound is the one in manganese chloride, manganous hydroxide, manganese carbonate, manganese nitrate, manganese dioxide.
CN201410208969.8A 2014-05-18 2014-05-18 Multielement doped lithium phosphate anode material and preparation method Pending CN104037411A (en)

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105428648A (en) * 2015-11-27 2016-03-23 中信大锰矿业有限责任公司大新锰矿分公司 Method for preparing battery cathode material lithium iron phosphate
CN105826536A (en) * 2016-05-19 2016-08-03 贵州安达科技能源股份有限公司 Lithium manganese ferric phosphate and preparing method thereof
CN105870420A (en) * 2016-05-27 2016-08-17 天津巴莫科技股份有限公司 Lithium-manganese-phosphate anode material for lithium-ion power battery and preparing method thereof
CN106505192A (en) * 2016-12-15 2017-03-15 钦州市钦南区科学技术情报研究所 A kind of iron manganese phosphate for lithium composite and preparation method thereof
CN104347853B (en) * 2014-09-24 2017-04-12 秦皇岛中科远达电池材料有限公司 Lithium manganate composite positive electrode material, a preparing method thereof and a lithium-ion battery
CN106784696A (en) * 2016-12-26 2017-05-31 深圳市贝特瑞纳米科技有限公司 A kind of titanium phosphate sodium/carbon composite, Preparation Method And The Use
CN108511700A (en) * 2018-01-23 2018-09-07 四川大学 Mostly metal-doped lithium iron phosphate/carbon composite material and preparation method
CN109678127A (en) * 2018-12-06 2019-04-26 绵阳天明新能源科技有限公司 A kind of titanium phosphate manganese iron and preparation method thereof
CN114538400A (en) * 2020-11-24 2022-05-27 天津理工大学 Multi-cation substituted phosphate electrode material and preparation method thereof
CN116443842A (en) * 2023-04-18 2023-07-18 东莞市创明电池技术有限公司 Fluorine-doped porous lithium iron manganese phosphate, preparation method thereof, positive electrode and battery
CN118373399A (en) * 2024-06-24 2024-07-23 湖南裕能新能源电池材料股份有限公司 Preparation method of lithium iron phosphate positive electrode material and lithium battery

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104347853B (en) * 2014-09-24 2017-04-12 秦皇岛中科远达电池材料有限公司 Lithium manganate composite positive electrode material, a preparing method thereof and a lithium-ion battery
CN105428648B (en) * 2015-11-27 2018-06-05 中信大锰矿业有限责任公司大新锰矿分公司 A kind of preparation method of battery anode material of lithium iron phosphate
CN105428648A (en) * 2015-11-27 2016-03-23 中信大锰矿业有限责任公司大新锰矿分公司 Method for preparing battery cathode material lithium iron phosphate
CN105826536A (en) * 2016-05-19 2016-08-03 贵州安达科技能源股份有限公司 Lithium manganese ferric phosphate and preparing method thereof
CN105870420A (en) * 2016-05-27 2016-08-17 天津巴莫科技股份有限公司 Lithium-manganese-phosphate anode material for lithium-ion power battery and preparing method thereof
CN105870420B (en) * 2016-05-27 2018-06-19 天津巴莫科技股份有限公司 A kind of lithium-ion-power cell manganese-lithium phosphate anode material and preparation method thereof
CN106505192A (en) * 2016-12-15 2017-03-15 钦州市钦南区科学技术情报研究所 A kind of iron manganese phosphate for lithium composite and preparation method thereof
CN106784696A (en) * 2016-12-26 2017-05-31 深圳市贝特瑞纳米科技有限公司 A kind of titanium phosphate sodium/carbon composite, Preparation Method And The Use
CN108511700A (en) * 2018-01-23 2018-09-07 四川大学 Mostly metal-doped lithium iron phosphate/carbon composite material and preparation method
CN108511700B (en) * 2018-01-23 2020-07-10 四川大学 Multi-metal doped lithium iron phosphate/carbon composite material and preparation method thereof
CN109678127A (en) * 2018-12-06 2019-04-26 绵阳天明新能源科技有限公司 A kind of titanium phosphate manganese iron and preparation method thereof
CN114538400A (en) * 2020-11-24 2022-05-27 天津理工大学 Multi-cation substituted phosphate electrode material and preparation method thereof
CN116443842A (en) * 2023-04-18 2023-07-18 东莞市创明电池技术有限公司 Fluorine-doped porous lithium iron manganese phosphate, preparation method thereof, positive electrode and battery
CN118373399A (en) * 2024-06-24 2024-07-23 湖南裕能新能源电池材料股份有限公司 Preparation method of lithium iron phosphate positive electrode material and lithium battery

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