CN108155368A - A kind of preparation method of carbon coating lithium manganese phosphate nanometer rods - Google Patents

A kind of preparation method of carbon coating lithium manganese phosphate nanometer rods Download PDF

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CN108155368A
CN108155368A CN201711478015.9A CN201711478015A CN108155368A CN 108155368 A CN108155368 A CN 108155368A CN 201711478015 A CN201711478015 A CN 201711478015A CN 108155368 A CN108155368 A CN 108155368A
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manganese phosphate
nanometer rods
lithium manganese
carbon coating
preparation
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裴波
胡棋威
卢北虎
刘飞
金鑫
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Wuhan Institute of Marine Electric Propulsion China Shipbuilding Industry Corp No 712 Institute CSIC
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Wuhan Institute of Marine Electric Propulsion China Shipbuilding Industry Corp No 712 Institute CSIC
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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
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • H01M4/58—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
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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 Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
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  • Crystallography & Structural Chemistry (AREA)
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Abstract

The invention discloses a kind of preparation methods of carbon coating lithium manganese phosphate nanometer rods, and MnSO is first added in into the beaker for fill distilled water4·H2O、H3PO4、LiOH∙H2O, surfactant and ascorbic acid after stirring a period of time, are transferred in autoclave, confined reaction for a period of time, washs after natural cooling, and precursor A is obtained after dry, carbon source is dissolved in distilled water, precursor A is added in, forms slurries B, slurries B ultrasound sound is stirred, then it is dried to obtain mixture C, after mixture C grinding uniformly, calcined under a nitrogen atmosphere to get to the carbon coating lithium manganese phosphate nanometer rods using the pattern of calcine by steps；Preparation method of the present invention is simple for process, is easily achieved, and moderate cost, also helps and shortens lithium ion diffusion path, enhancing electrode reaction, so as to improve the chemical property of anode material for lithium-ion batteries.

Description

A kind of preparation method of carbon coating lithium manganese phosphate nanometer rods
Technical field
The invention belongs to lithium-ion technology and new material synthesis fields, and in particular to a kind of lithium ion battery carbon coating phosphorus The preparation method of sour manganese lithium nanometer rods positive electrode.
Background technology
In recent years, people start increasingly to pay close attention to higher performance and cheap rechargeable lithium ion batteries in electronics Application in equipment.Since phosphate of olivine type LiMPO in 19974(M=Fe, Mn, Co, Ni) is by report can conduct for the first time Since anode material for lithium-ion batteries, lithium manganese phosphate（LiMnPO4）Due to its cheap, environmental-friendly, nontoxic, cycle performance Well, high theoretical specific capacity (170 mAh g-1) and the advantages that charge and discharge platform and be widely studied.But in LiMnPO4 In crystal structure, because of the good FeO of electric conductivity6The PO that octahedron is almost insulated4 3-Separation, reduces LiMnPO4Lead Electrically, the hexagonal closest packing of oxygen atom three-dimensional limits Li+Diffusion.Therefore, low conductivity and slow lithium from Son diffusion limits LiMnPO4One important parameter of high rate performance-high-power applications of positive electrode.
Based on this, many researchers are dedicated to overcome thing problems, such as these in recent years, have done the work of following three aspect：It improves The conductivity on surface（It is coated by conductive agent）；Increase the conductivity of lithium ion（It is adulterated by metal cation）With shorten lithium from The transmission path of son（By the particle size for reducing material）.
Isam etc. is reported in rhombic system, Pnma space groups, and lithium ion preferentially along b axis directions spread by selection, without It is a axis and the diffusion of c-axis direction, because lithium ion is along migration energy of the b axis directions diffusion with minimum.The uses such as Gaberscek One theoretical model, explains in LiMPO4Why ionic conductivity is than electronic conductance in (M=Fe, Mn, Co, Ni) crystal Rate is much smaller, shows the diffusion of lithium ion for improving LiMPO4It is non-in terms of the dynamics of (M=Fe, Mn, Co, Ni) positive electrode Chang Guanjian.Therefore, in order to improve LiMnPO4The kinetic factor of positive electrode, scholars propose a possible approach and lead to Cross regulation and control LiMnPO4The micro- knot of positive electrode enough shortens the size along b axis directions, and this material is because that can reduce lithium ion diffusion road Diameter and with very excellent high rate capability.Recently, many scholars make great progress in this respect.For example, using heat Decomposition method, by adjusting manganese source concentration, LiMnPO4Material is from nano bar-shape（It is about 30-50 nm along b axis directions）It is changed into and receives Rice sheet.It uses solvent-thermal method, LiMnPO is prepared as solvent using N-Methyl pyrrolidone and graphite oxide solution4Nano sheet material Material/graphene composite material（It is about 20-70 nm along b axis directions）, which is about 159 mAh g in the specific capacity of 0.05 C-1。
In addition, in LiMnPO4The agent of material surface coated with conductive can not only improve electric conductivity and reduce the polarization of battery, but also can Think LiMnPO4Electron tunnel is provided, for compensating Li+Charge balance during deintercalation.
Invention content
The object of the present invention is to provide a kind of preparation method of carbon coating lithium manganese phosphate nanometer rods, this method is conducive to shorten Lithium ion diffusion path, enhancing electrode reaction, so as to improve the chemical property of anode material for lithium-ion batteries.
The technical solution adopted by the present invention to solve the technical problems is：A kind of preparation of carbon coating lithium manganese phosphate nanometer rods Method includes the following steps
a）, MnSO is added in into the beaker for fill distilled water4·H2O、H3PO4、LiOH∙H2O, surfactant and ascorbic acid, After stirring a period of time, it is transferred in autoclave；
b）, confined reaction for a period of time, washed after natural cooling, precursor A obtained after dry；
c）, carbon source is dissolved in distilled water, add in precursor A, form slurries B；
d）, by slurries B ultrasound sound stir, be then dried to obtain mixture C；
e）, by after mixture C grinding uniformly, calcined under a nitrogen atmosphere to get to the carbon packet using the pattern of calcine by steps Cover lithium manganese phosphate nanometer rods.
A kind of preparation method of carbon coating lithium manganese phosphate nanometer rods, MnSO4·H2O dosages are 40 mL distilled water 5—30mmol.Its H3PO4Dosage is 40 5-30mmol of mL distilled water.Its LiOH H2O dosages for 40 mL distilled water 10- 120mmol.Its ascorbic acid dosage is 40 1-15mmol of mL distilled water.Its surfactant for neopelex or Polyethylene glycol, dosage are 40 0.1-3mmol of mL distilled water.
A kind of preparation method of carbon coating lithium manganese phosphate nanometer rods, step b）Middle confined reaction temperature is 120-250 DEG C, the reaction time be 12-36h, follow-up drying temperature be 50-100 DEG C, drying time be 5-20h.
A kind of preparation method of carbon coating lithium manganese phosphate nanometer rods, step c）Middle carbon source is sucrose or grape Sugar, the dosage of corresponding 2000mg lithium manganese phosphate precursor As is 100-700mg.
A kind of preparation method of carbon coating lithium manganese phosphate nanometer rods, step d）The drying temperature of middle slurries B is 70-150 DEG C, drying time be 4-18h.
A kind of preparation method of carbon coating lithium manganese phosphate nanometer rods, step e）Middle calcine by steps pattern be with 2—7℃ min-1Heating rate 200-400 DEG C calcine 2-8h, then with 1-5 DEG C of min-1Heating rate exist 400-800 DEG C of 5-12h of calcining.
The beneficial effects of the invention are as follows：Preparation method of the present invention is simple for process, is easily achieved, and moderate cost, in addition Preparation method of the present invention, which also helps, shortens lithium ion diffusion path, enhancing electrode reaction, so as to improve lithium ion cell positive The chemical property of material.
Description of the drawings
Fig. 1 is the stereoscan photograph of carbon coating lithium manganese phosphate nanometer rods in the embodiment of the present invention 1；
Fig. 2 is the transmission electron microscope photo of carbon coating lithium manganese phosphate nanometer rods in the embodiment of the present invention 1；
Fig. 3 is charging and discharging curve of the carbon coating lithium manganese phosphate nanometer rods under 0.1,5C current densities in the embodiment of the present invention 1（Electricity Ranging from 2.5-4.2V is pressed, defines 1C=170mAg-1）.
Specific embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings.
Most currently used conductive agent is various carbon sources, uses solvent thermal reaction, with CH3COOLi、Mn（CH3COO）2With H3PO4It is raw material, oleamide as solvent and carbon source, first prepares LiMnPO4/ C presomas, then by later stage high-temperature calcination, i.e., The good LiMnPO of crystallinity is made4/ C, the specific capacity under 0.1 C discharge-rates are 168 mAh g-1, the electric discharge under 5C Specific capacity is still up to 105 mAh g-1.Using spray heating decomposition, after the reactant predecomposition stoichiometrically mixed, so It afterwards with acetylene black mixing and ball milling, is finally sintered under 500 DEG C of reducing atmosphere, obtains LiMnPO with good conductivity4/ C, Specific capacity under 0.1 C discharge-rates is 147mAh g-1, the specific discharge capacity under 1 C is still up to 145 mAh g-1
Referring to figs. 1 to shown in Fig. 3, the present invention is preparing lithium manganese phosphate lithium ion battery just using hydro-thermal reaction with surfactant Pole material is obtained along the controllable nanometer rods of b axis direction sizes, and the specific discharge capacity and high rate performance of lithium manganese phosphate exist with material The reduction of b axis direction sizes and improve, shorten its size and increase in b axis directions（010）The area in face is conducive to shorten lithium Ion diffusion path, enhancing electrode reaction, so as to improve the chemical property of carbon coating lithium manganese phosphate composite material.
Embodiment 1
a）15 mmol MnSO are added in into the beaker for filling 40 mL distilled water4·H2O、15 mmol H3PO4、45 mmol LiOH∙H2O, after stirring 20 min, it is anti-to be transferred to high pressure for 0.6 mmol neopelexes and 7.5 mmol ascorbic acid It answers in kettle；
b）Confined reaction for 24 hours, washs after natural cooling at 170 DEG C, and dry 12h, obtains precursor A at 60 DEG C；
c）200mg sucrose is dissolved in 4mL distilled water, adds in 2000mg precursor As, forms slurries B；
d）After slurries B ultrasound sound is stirred 15 min, dry 12h obtains mixture C at 90 DEG C；
e）After said mixture C grindings uniformly, calcine under a nitrogen atmosphere.Using the pattern of calcine by steps, with 4 DEG C of min-1 Heating rate 350 DEG C calcine 4h, then with 2 DEG C of min-1Heating rate 9h are calcined at 650 DEG C to get to the carbon packet Cover lithium manganese phosphate nanometer rods.
Embodiment 2
a）30 mmol MnSO are added in into the beaker for filling 40 mL distilled water4·H2O、30 mmol H3PO4、90 mmol LiOH∙H2O, 1.5 mmol polyethylene glycol and 15 mmol ascorbic acid after stirring 20 min, are transferred in autoclave；
b）36 h of confined reaction, is washed after natural cooling at 220 DEG C, and dry 15 h, obtain precursor A at 80 DEG C；
c）450 mg sucrose are dissolved in 4mL distilled water, add in 2000 mg precursor As, form slurries B；
d）After slurries B ultrasound sound is stirred 15 min, dry 8 h obtain mixture C at 120 DEG C；
e）After said mixture C grindings uniformly, calcine under a nitrogen atmosphere, using the pattern of calcine by steps, with 3 DEG C of min-1 Heating rate 400 DEG C calcine 7 h, then with 5 DEG C of min-1Heating rate 5 h are calcined at 800 DEG C to get to the carbon Coat lithium manganese phosphate nanometer rods.
Embodiment 3
a）5 mmol MnSO are added in into the beaker for filling 40 mL distilled water4·H2O、5 mmol H3PO4、10 mmol LiOH ∙H2O, 0.1 mmol neopelexes and 1 mmol ascorbic acid after stirring 20 min, are transferred to autoclave In；
b）Confined reaction 12h, is washed after natural cooling at 120 DEG C, and dry 20h, obtains precursor A at 50 DEG C；
c）100mg glucose is dissolved in 4mL distilled water, adds in 2000mg precursor As, forms slurries B；
d）After slurries B ultrasound sound is stirred 15 min, dry 18h obtains mixture C at 70 DEG C；
e）After said mixture C grindings uniformly, calcine under a nitrogen atmosphere.Using the pattern of calcine by steps, with 2 DEG C of min-1 Heating rate 200 DEG C calcine 8h, then with 1 DEG C of min-1Heating rate 7h are calcined at 400 DEG C to get to the carbon packet Cover lithium manganese phosphate nanometer rods.
Embodiment 4
a）5 mmol MnSO are added in into the beaker for filling 40 mL distilled water4·H2O、5 mmol H3PO4、120 mmol LiOH∙H2O, 3 mmol polyethylene glycol and 1 mmol ascorbic acid after stirring 20 min, are transferred in autoclave；
b）Confined reaction 36h, is washed after natural cooling at 250 DEG C, and dry 5h, obtains precursor A at 100 DEG C；
c）700mg glucose is dissolved in 4mL distilled water, adds in 2000mg precursor As, forms slurries B；
d）After slurries B ultrasound sound is stirred 15 min, dry 4h obtains mixture C at 150 DEG C；
e）After said mixture C grindings uniformly, calcine under a nitrogen atmosphere.Using the pattern of calcine by steps, with 7 DEG C of min-1 Heating rate 200 DEG C calcine 2h, then with 1 DEG C of min-1Heating rate 12h are calcined at 400 DEG C to get to the carbon packet Cover lithium manganese phosphate nanometer rods.
The embodiment that the above-described embodiments merely illustrate the principles and effects of the present invention and part uses, for For those of ordinary skill in the art, without departing from the concept of the premise of the invention, can also make it is several deformation and It improves, these belong to protection scope of the present invention.

Claims (10)

1. a kind of preparation method of carbon coating lithium manganese phosphate nanometer rods, it is characterised in that：Include the following steps
a）, MnSO is added in into the beaker for fill distilled water4·H2O、H3PO4、LiOH•H2O, surfactant and ascorbic acid, After stirring a period of time, it is transferred in autoclave；
b）, confined reaction for a period of time, washed after natural cooling, precursor A obtained after dry；
c）, carbon source is dissolved in distilled water, add in precursor A, form slurries B；
d）, by slurries B ultrasound sound stir, be then dried to obtain mixture C；
e）, by after mixture C grinding uniformly, calcined under a nitrogen atmosphere to get to carbon coating phosphorus using the pattern of calcine by steps Sour manganese lithium nanometer rods.
2. the preparation method of a kind of carbon coating lithium manganese phosphate nanometer rods according to claim 1, which is characterized in that described MnSO4·H2O dosages are 40 5-30mmol of mL distilled water.
3. the preparation method of a kind of carbon coating lithium manganese phosphate nanometer rods according to claim 1, which is characterized in that described H3PO4Dosage is 40 5-30mmol of mL distilled water.
4. the preparation method of a kind of carbon coating lithium manganese phosphate nanometer rods according to claim 1, which is characterized in that described LiOH∙H2O dosages are 40 10-120mmol of mL distilled water.
5. the preparation method of a kind of carbon coating lithium manganese phosphate nanometer rods according to claim 1, which is characterized in that described Surfactant is neopelex or polyethylene glycol, and dosage is 40 0.1-3mmol of mL distilled water.
6. the preparation method of a kind of carbon coating lithium manganese phosphate nanometer rods according to claim 1, which is characterized in that described Ascorbic acid dosage is 40 1-15mmol of mL distilled water.
7. the preparation method of a kind of carbon coating lithium manganese phosphate nanometer rods according to claim 1, which is characterized in that described Step b）Middle confined reaction temperature is 120-250 DEG C, the reaction time is 12-36h, and follow-up drying temperature is 50-100 DEG C, does The dry time is 5-20h.
8. the preparation method of a kind of carbon coating lithium manganese phosphate nanometer rods according to claim 1, which is characterized in that described Step c）Middle carbon source is sucrose or glucose, and the dosage of corresponding 2000mg lithium manganese phosphate precursor As is 100-700mg.
9. the preparation method of a kind of carbon coating lithium manganese phosphate nanometer rods according to claim 1, which is characterized in that described Step d）The drying temperature of middle slurries B is 70-150 DEG C, drying time is 4-18h.
10. the preparation method of a kind of carbon coating lithium manganese phosphate nanometer rods according to claim 1, which is characterized in that described Step e）Middle calcine by steps pattern is with 2-7 DEG C of min-1Heating rate 200-400 DEG C calcine 2-8h, then with 1—5℃ min-1Heating rate 400-800 DEG C calcine 5-12h.
CN201711478015.9A 2017-12-29 2017-12-29 A kind of preparation method of carbon coating lithium manganese phosphate nanometer rods Pending CN108155368A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114669311A (en) * 2022-03-17 2022-06-28 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） Composite catalyst and preparation method and application thereof

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Publication number Priority date Publication date Assignee Title
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CN102299334A (en) * 2011-07-15 2011-12-28 北京化工大学 Carbon coated LiFePO4 porous anode and preparation method thereof
CN104064773A (en) * 2014-07-07 2014-09-24 盐城市新能源化学储能与动力电源研究中心 Preparation method of carbon-coated lithium manganese borate cathode material for lithium ion battery
CN106340624A (en) * 2016-09-29 2017-01-18 武汉船用电力推进装置研究所（中国船舶重工集团公司第七二研究所） Preparation method of carbon coated LiFePO4 nanorods

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102054986A (en) * 2010-11-16 2011-05-11 中国科学院宁波材料技术与工程研究所 Ultrahigh-capacity lithium ion battery anode material prepared by microwave method and preparation method thereof
CN102299334A (en) * 2011-07-15 2011-12-28 北京化工大学 Carbon coated LiFePO4 porous anode and preparation method thereof
CN104064773A (en) * 2014-07-07 2014-09-24 盐城市新能源化学储能与动力电源研究中心 Preparation method of carbon-coated lithium manganese borate cathode material for lithium ion battery
CN106340624A (en) * 2016-09-29 2017-01-18 武汉船用电力推进装置研究所（中国船舶重工集团公司第七二研究所） Preparation method of carbon coated LiFePO4 nanorods

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114669311A (en) * 2022-03-17 2022-06-28 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） Composite catalyst and preparation method and application thereof
CN114669311B (en) * 2022-03-17 2023-08-15 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） Composite catalyst and preparation method and application thereof

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