CN107482181B - Composite lithium ion battery anode material Li3V2(PO4)3/C and preparation method thereof - Google Patents

Composite lithium ion battery anode material Li3V2(PO4)3/C and preparation method thereof Download PDF

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CN107482181B
CN107482181B CN201710557875.5A CN201710557875A CN107482181B CN 107482181 B CN107482181 B CN 107482181B CN 201710557875 A CN201710557875 A CN 201710557875A CN 107482181 B CN107482181 B CN 107482181B
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li3v2
beaker
deionized water
lithium
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CN107482181A (en
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倪世兵
唐俊
康桃
杨学林
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China Three Gorges University CTGU
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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
    • 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
    • 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
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • 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)
  • Engineering & Computer Science (AREA)
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  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
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Abstract

the invention provides a method for introducing carbon by an intermediate liquid phase to prepare a carbon composite lithium vanadium phosphate anode material, which comprises the specific steps of weighing a lithium source and a vanadium source in a small beaker, adding deionized water, stirring for 20min until the lithium source and the vanadium source are completely dissolved, transferring the mixture into a hydrothermal liner, adding the deionized water to 80% of the volume of the liner, and carrying out hydrothermal treatment for 24-36 h in a blast oven at 120-160 ℃. Weighing a phosphorus source and an organic carbon source in a beaker, adding deionized water, stirring for 20min until the phosphorus source and the organic carbon source are completely dissolved, then slowly dropwise adding the naturally-cooled intermediate phase liquid into the beaker in which the phosphorus source and the organic carbon source are dissolved, and stirring for 20min until the solution becomes orange yellow. And then, drying the liquid-phase precursor in a forced air oven at 65 ℃ for 24-36 h until the precursor is completely dried. And pre-burning the obtained green-coated precursor powder at 350 ℃ for 4-6 h in a nitrogen atmosphere, calcining at 700-800 ℃ for 6-10 h, and naturally cooling to obtain the Li3V2(PO4)3/C composite material which is used as the lithium ion battery anode material and shows better electrochemical performance.

Description

Composite lithium ion battery anode material Li3V2(PO4)3/C and preparation method thereof
Technical Field
The invention relates to a high-performance lithium ion battery anode material, in particular to a preparation method of a Li3V2(PO4)3/C composite material, and belongs to the field of electrochemical power sources.
Technical Field
The lithium ion battery has been widely applied to portable electronic products, hybrid vehicles, pure power vehicles and large energy storage devices at present due to the advantages of high specific energy, low self-discharge, long service life, no memory effect, environmental friendliness and the like, and is dominant in the current energy storage market. With the application of a large number of lithium ion batteries, the market puts higher requirements on the performance of the lithium ion batteries.
The electrode material is used as the core and key technology of the lithium ion battery, and determines the comprehensive performance of the lithium ion battery. And among the four parts of the lithium ion battery, the cost of the anode material is the highest and is 30-40%. Therefore, the development of the cathode material plays a key role in reducing the cost of the battery and improving the electrochemical performance of the battery. At present, the widely used anode materials mainly include lithium cobaltate, lithium manganate, lithium iron phosphate and ternary materials. Among them, lithium cobaltate is difficult to prepare, has poor safety, is toxic and is expensive. The lithium manganate has good safety, but low capacity, a john-Teller effect and poor cycle stability. The lithium iron phosphate is high in safety, good in cycling stability and long in cycling life, but low in energy density, poor in low-temperature performance and low in discharge platform. The ternary material has high energy density and good cycle stability, but the first charge and discharge efficiency is not high, the thermal stability is not good, and the phase change is easy to occur, so that further research is needed.
Compared with other lithium ion cathode materials, the Li3V2(PO4)3 material has higher charge and discharge platforms and reversible capacity (the theoretical capacity is 133mAh g < -1 > at a voltage of 3-4.3V, and is 197mAh g < -1 > at a voltage of 3-4.8V). Li3V2(PO4)3 as a polyanion compound has better thermal stability, lower cost and long cycle life. Based on the above research, Li3V2(PO4)3 has become a positive electrode material of lithium ion batteries with application potential in recent years.
Disclosure of Invention
The invention provides a preparation process of Li3V2(PO4) 3/C. Introducing a carbon source into the intermediate phase liquid, inducing the organic carbon source molecules to be adsorbed on the surfaces of the intermediate phase liquid by using the crystallization of the intermediate phase liquid in the drying process, and carbonizing the organic carbon source molecules in situ along the surfaces of Li3V2(PO4)3 while forming Li3V2(PO4)3 in the subsequent solid phase reaction. On one hand, the Li3V2(PO4)3 and C are favorably and uniformly compounded on a microscopic scale, and the conductivity of the material is remarkably improved; on the other hand, C can effectively inhibit the growth of Li3V2(PO4)3 grains and ensure high lithium ion diffusion efficiency. Finally, the prepared Li3V2(PO4)3/C as the positive electrode of the lithium ion battery shows excellent electrochemical performance.
the invention relates to a preparation method of a lithium ion battery anode material, which is a Li3V2(PO4)3/C composite material, is in a composite shape and consists of Li3V2(PO4)3 particles with the size of about 100nm and sheets with the size of about 1 mu m. The preparation method comprises the following steps: dissolving a certain amount of lithium source, vanadium source and hexamethylenetetramine in a small beaker filled with 20mL of deionized water, and stirring for 30min until the lithium source, the vanadium source and the hexamethylenetetramine are fully dissolved; and transferring the obtained mixed solution into a hydrothermal inner container, adding deionized water to 80% of the volume of the inner container, carrying out hydrothermal treatment in a blast oven at 120-160 ℃ for 24-36 h, and naturally cooling to obtain an intermediate phase liquid. Weighing a certain amount of carbon source and phosphorus source, dissolving the carbon source and the phosphorus source in a beaker filled with 20mL of deionized water, stirring for 20min until the carbon source and the phosphorus source are fully dissolved, then slowly dropwise adding the cooled intermediate phase liquid into the beaker, and stirring for 30min after the dropwise adding is finished until the color is orange yellow. And then, placing the beaker in a 65 ℃ air blast oven to be dried for 24-36 h until the beaker is completely dried. And pre-burning the dried precursor powder at 350 ℃ for 4-6 h in a nitrogen atmosphere, and calcining at 700-800 ℃ for 6-10 h. After cooling, the Li3V2(PO4)3/C composite material is obtained.
The molar ratio of the lithium, the vanadium, the phosphorus and the hexamethylene tetramine is 3: 2: 3: 2 to 10. The carbon source accounts for 0-15% of the total mass. The lithium source is lithium carbonate, lithium hydroxide, lithium acetate or lithium oxalate, the vanadium source is vanadium pentoxide or ammonium metavanadate, the phosphorus source is ammonium dihydrogen phosphate, diammonium hydrogen phosphate or ammonium phosphate, and the carbon source is citric acid, glucose, sucrose or ascorbic acid.
The preparation method, the material and the performance of the Li3V2(PO4)3/C composite material have the following remarkable characteristics:
(1) The synthesis process is simple, easy to operate, good in repeatability and low in cost;
(2) The synthesized intermediate phase is a liquid phase, so that the uniformity of the material can be obviously enhanced;
(3) The prepared carbon composite Li3V2(PO4)3 material has a composite morphology and is composed of Li3V2(PO4)3 particles with the size of about 100nm and sheets with the size of about 1 mu m;
(4) The Li3V2(PO4)3/C composite material prepared by the invention is used as the anode material of the lithium ion battery and shows better cycle performance and higher specific capacity.
Drawings
Figure 1 XRD pattern of the sample prepared in example 1.
FIG. 2 SEM image of sample prepared in example 1.
Fig. 3 graph (a) of the first three charge and discharge curves and graph (b) of the cycle performance of the sample prepared in example 1.
FIG. 4 is a graph of the cycle performance of the samples prepared in example 2.
FIG. 5 cycle performance plot of the samples prepared in example 3.
Detailed Description
example 1
Weighing 3mmol of lithium carbonate, 2mmol of vanadium pentoxide and 5mmol of hexamethylenetetramine, dissolving in a small beaker filled with 20mL of deionized water, and stirring for 30min until the lithium carbonate, the vanadium pentoxide and the hexamethylenetetramine are fully dissolved; and transferring the obtained mixed solution into a hydrothermal liner, adding deionized water to 80% of the volume of the liner, performing hydrothermal treatment in a blast oven at 120 ℃ for 24 hours, and naturally cooling to obtain intermediate phase liquid. Weighing 0.05g of citric acid and 6mmol of ammonium dihydrogen phosphate, dissolving in a beaker filled with 20mL of deionized water, stirring for 20min until the citric acid and the ammonium dihydrogen phosphate are fully dissolved, then slowly dropwise adding the cooled intermediate phase liquid into the beaker, and stirring for 30min after the dropwise adding is finished until the color is orange yellow. The beaker was then placed in a forced air oven at 65 ℃ for 36h to dry completely. And placing the dried precursor powder in a nitrogen atmosphere for presintering at 350 ℃ for 4h and calcining at 750 ℃ for 8 h. After cooling, the Li3V2(PO4)3/C composite material is obtained. The XRD pattern analysis of the prepared sample showed that all diffraction peaks corresponded to Li3V2(PO4)3 (No. ✩, XRD card JCPDS, No. 01-072-7074) as shown in FIG. 1, indicating that the Li3V2(PO4)3 sample was successfully prepared. The sample was subjected to SEM characterization, and as can be seen from FIG. 2, Li3V2(PO4)3/C has a composite morphology consisting of Li3V2(PO4)3 particles with a size of about 100nm and platelets with a size of about 1 μm. The Li3V2(PO4)3 composite material obtained in the above step was coated on an aluminum foil (7.5:1.5:1, Li3V2(PO4) 3/C: acetylene black: PVDF), cut into 14mm round pieces, and vacuum-dried at 120 ℃ for 12 hours. A metal lithium sheet is used as a counter electrode, a Celgard membrane is used as a diaphragm, a solution of EC + DEC (volume ratio of 1:1) dissolved with LiPF6 (1mol/L) is used as an electrolyte, and the CR2025 type battery is assembled in a glove box protected by argon. And standing for 8 hours after the battery is assembled, and then performing constant-current charging and discharging tests by using a CT2001A battery test system, wherein the test voltage is 3-4.3V. FIG. 3 shows that the first charge and discharge capacities of the Li3V2(PO4)3/C electrode prepared in example 1 were 143.4 and 114.3mAh/g, respectively, and the charge and discharge capacities after 90 cycles were 113.5 and 112.7 mAh/g, respectively, showing better electrochemical properties.
Example 2
Weighing 3mmol of lithium acetate, 2mmol of vanadium pentoxide and 5mmol of hexamethylenetetramine, dissolving in a small beaker filled with 20mL of deionized water, and stirring for 30min until the lithium acetate, the vanadium pentoxide and the hexamethylenetetramine are fully dissolved; and transferring the obtained mixed solution into a hydrothermal liner, adding deionized water to 80% of the volume of the liner, performing hydrothermal treatment in a blast oven at 120 ℃ for 24 hours, and naturally cooling to obtain intermediate phase liquid. 0.05g of glucose and 6mmol of ammonium dihydrogen phosphate are weighed and dissolved in a beaker filled with 20mL of deionized water, stirred for 20min until the glucose and the ammonium dihydrogen phosphate are fully dissolved, then the cooled intermediate phase liquid is slowly dripped into the beaker, and stirred for 30min after the dripping is finished until the color is orange yellow. The beaker was then placed in a forced air oven at 65 ℃ for 36h to dry completely. And placing the dried precursor powder in a nitrogen atmosphere for presintering at 350 ℃ for 4h and calcining at 750 ℃ for 8 h. After cooling, the Li3V2(PO4)3/C composite material is obtained. An electrode was prepared and a battery was assembled in the same manner as in example 1. FIG. 4 shows that the first charge and discharge capacities of the Li3V2(PO4)3/C electrode prepared in example 2 were 130.4 and 120.2 mAh/g, respectively, and the charge and discharge capacities after 90 cycles were 116.5 and 115.5 mAh/g, respectively, showing better electrochemical properties.
Example 3
Weighing 3mmol of lithium hydroxide, 2mmol of ammonium metavanadate and 5mmol of hexamethylenetetramine, dissolving in a small beaker filled with 20mL of deionized water, and stirring for 30min until the lithium hydroxide, the ammonium metavanadate and the hexamethylenetetramine are fully dissolved; and transferring the obtained mixed solution into a hydrothermal liner, adding deionized water to 80% of the volume of the liner, performing hydrothermal treatment in a blast oven at 120 ℃ for 24 hours, and naturally cooling to obtain intermediate phase liquid. 0.05g of sucrose and 6mmol of ammonium dihydrogen phosphate are weighed and dissolved in a beaker filled with 20mL of deionized water, stirred for 20min until the sucrose and the ammonium dihydrogen phosphate are fully dissolved, then the cooled intermediate phase liquid is slowly dripped into the beaker, and stirred for 30min after the dripping is finished until the color is orange yellow. The beaker was then placed in a forced air oven at 65 ℃ for 36h to dry completely. And placing the dried precursor powder in a nitrogen atmosphere for presintering at 350 ℃ for 4h and calcining at 750 ℃ for 8 h. After cooling, the Li3V2(PO4)3/C composite material is obtained. An electrode was prepared and a battery was assembled in the same manner as in example 1. FIG. 5 shows that the first charge and discharge capacities of the Li3V2(PO4)3/C electrode prepared in example 3 were 133.3 and 111.4 mAh/g, respectively, and the charge and discharge capacities after 90 cycles were 109.3 and 108.5 mAh/g, respectively, showing better electrochemical properties.

Claims (1)

1. A preparation method of a lithium ion battery anode Li3V2(PO4)3/C composite material is characterized in that 3mmol of lithium carbonate, 2mmol of vanadium pentoxide and 5mmol of hexamethylenetetramine are weighed and dissolved in a small beaker filled with 20mL of deionized water, and the mixture is stirred for 30min until the lithium ion battery anode Li3V2(PO4)3/C composite material is fully dissolved; transferring the obtained mixed solution into a hydrothermal liner, adding deionized water to 80% of the volume of the liner, performing hydrothermal treatment in a blast oven at 120 ℃ for 24 hours, and naturally cooling to obtain a mesophase liquid; weighing 0.05g of citric acid and 6mmol of ammonium dihydrogen phosphate, dissolving in a beaker filled with 20mL of deionized water, stirring for 20min until the citric acid and the ammonium dihydrogen phosphate are fully dissolved, then slowly dropwise adding the cooled intermediate phase liquid into the beaker, and stirring for 30min after the dropwise adding is finished until the color is orange yellow; then placing the beaker in a forced air oven at 65 ℃ to be dried for 36h until the beaker is completely dried; presintering the dried precursor powder at 350 ℃ for 4h in a nitrogen atmosphere, and calcining at 750 ℃ for 8 h; after cooling, the Li3V2(PO4)3/C composite material is obtained.
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CN108550845B (en) * 2018-04-18 2020-10-30 华中科技大学 Application of lithium vanadium phosphate sodium material and low-temperature battery thereof
CN113699687B (en) * 2021-08-18 2022-08-05 三峡大学 Double-needle electrostatic spinning Li 3 VO 4 Preparation method of/C fiber lithium ion battery cathode material

Citations (4)

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Publication number Priority date Publication date Assignee Title
CN102386412A (en) * 2011-11-11 2012-03-21 中南大学 Lithium ion battery anode Li3V2(PO4)3/C composite material and preparation method thereof
CN104201363A (en) * 2014-07-01 2014-12-10 三峡大学 Carbon-coated Li3VO4 lithium ion battery anode material and preparation method thereof
CN104466176A (en) * 2014-11-07 2015-03-25 哈尔滨工业大学 Preparation method of lithium ion battery positive electrode material Li3V2(PO4)3
CN104779393A (en) * 2015-04-15 2015-07-15 河北民族师范学院 Method for preparing lithium-vanadium-phosphate lithium ion battery positive material by means of liquid phase reduction

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102386412A (en) * 2011-11-11 2012-03-21 中南大学 Lithium ion battery anode Li3V2(PO4)3/C composite material and preparation method thereof
CN104201363A (en) * 2014-07-01 2014-12-10 三峡大学 Carbon-coated Li3VO4 lithium ion battery anode material and preparation method thereof
CN104466176A (en) * 2014-11-07 2015-03-25 哈尔滨工业大学 Preparation method of lithium ion battery positive electrode material Li3V2(PO4)3
CN104779393A (en) * 2015-04-15 2015-07-15 河北民族师范学院 Method for preparing lithium-vanadium-phosphate lithium ion battery positive material by means of liquid phase reduction

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