CN105552353A - Negative electrode Bi2WO6/C composite material of high-performance lithium ion battery and preparation method of negative electrode Bi2WO6/C composite material - Google Patents

Negative electrode Bi2WO6/C composite material of high-performance lithium ion battery and preparation method of negative electrode Bi2WO6/C composite material Download PDF

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CN105552353A
CN105552353A CN201610077248.7A CN201610077248A CN105552353A CN 105552353 A CN105552353 A CN 105552353A CN 201610077248 A CN201610077248 A CN 201610077248A CN 105552353 A CN105552353 A CN 105552353A
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bi2wo6
composite material
lithium ion
composite
ion battery
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CN105552353B (en
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张林森
王力臻
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Zhengzhou University of Light Industry
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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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • 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)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention relates to a negative electrode Bi2WO6/C composite material of a high-performance lithium ion battery and a preparation method of the negative electrode Bi2WO6/C composite material. In the negative electrode Bi2WO6 composite material, spherical-like Bi2WO6 particles are coated with C. The preparation method comprises the following steps of firstly, jointly adding Bi(NO<3>)<3>.5H<2>O serving as a bismuth source and Na<2>WO<4>.2H<2>O serving as a tungsten source into a mixed solution of ethylene glycol and ethyl alcohol; secondly, adding urea and glucose; and finally, transferring the mixture liquid into a hydrothermal reaction kettle for reaction, and separating, washing and drying a product to obtain the Bi2WO6/C composite material. The Bi2WO6/C composite material prepared according to the invention has the characteristics of high electrochemical capacity, high cycle stability, excellent rate performance and the like, and is simple in the preparation process, high in repeatability and easy in industrial production.

Description

A kind of high performance lithium ionic cell cathode Bi 2wO 6/ C composite and preparation method thereof
Technical field
The present invention relates to technical field of lithium ion, be specifically related to a kind of high performance lithium ionic cell cathode Bi 2wO 6/ C composite and preparation method thereof.
Background technology
At present, the negative material that lithium ion battery adopts is all generally carbon materials, as graphite, soft carbon, hard carbon etc., although carbon negative pole material has some excellent characteristic, but also there is obvious shortcoming, as high in soft carbon first charge-discharge irreversible capacity, without obvious charge and discharge platform; Hard carbon first charge-discharge efficiency is low, without obvious first charge-discharge platform and the very large current potential that causes because of impure H delayed etc.Usually, the theoretical expression of compound that lithium is formed in material with carbon element is LiC 6, theoretical specific capacity stoichiometrically only has 372mAh/g, and its density is also smaller, causes its volume and capacity ratio very low.In addition, when charge and discharge potential reaches 0V or be lower, graphite electrode has lithium and be deposited generation dendrite, may barrier film be stung, cause battery plus-negative plate short circuit, thus there is potential safety hazard.So study high specific capacity, negative material that security performance is good, it is the inexorable trend of lithium ion battery technology development, particularly new type power lithium ion battery development.Compared with material with carbon element, Bi 2wO 6negative material as lithium ion battery has high specific capacity, makes it have very large development potentiality as lithium ion battery negative material of new generation, but Bi 2wO 6conductivity is poor, simultaneously Bi 2wO 6at Lithium-ion embeding/deviate from process, along with the expansion/contraction of volume, volume deformation is large, and the easy efflorescence of particle, have impact on cycle life.
Summary of the invention
The object of the invention is to solve the above-mentioned technical problem existed in prior art, a kind of high performance lithium ionic cell cathode Bi is provided 2wO 6/ C composite and preparation method thereof.
The object of the invention is to be achieved through the following technical solutions:
The present invention relates to a kind of lithium ion battery negative Bi 2wO 6/ C composite, described composite material comprises the spherical Bi of class 2wO 6and be evenly coated on such spherical Bi 2wO 6outside C coating layer, described Bi 2wO 6average grain diameter be 100nm ~ 3000nm, C content is 0.5 ~ 10%.Bi 2wO 6the less electro-chemical activity of/C composite particle diameter is higher, but after being less than 100nm, material is easily reunited, and affects the electrode coating process of battery; The larger electro-chemical activity of composite material particle diameter is lower, and therefore unsuitable excessive, particle diameter is less than 3000nm.C content is less than after 0.5%, Bi 2wO 6the conductivity of/C composite is poor, and meanwhile, C is to Bi 2wO 6the inhibition of volumetric expansion is poor; C content is greater than after 10%, Bi 2wO 6the middle Bi of/C composite 2wO 6content reduces, Bi 2wO 6/ C composite specific capacity declines.
At Bi of the present invention 2wO 6in/C composite, carbon improves Bi 2wO 6conductance, can cushion Bi simultaneously 2wO 6volumetric expansion in lithium ion battery charge and discharge process, extends its cycle life.
The invention still further relates to a kind of high performance lithium ionic cell cathode Bi 2wO 6the preparation method of/C composite, described method comprises the steps:
S1, be the Bi (NO of 2:1 by mol ratio 3) 35H 2o and Na 2wO 42H 2o joins in the mixed solution of ethylene glycol and absolute ethyl alcohol, wherein, and Bi (NO 3) 35H 2the mol ratio of O and ethylene glycol is 1:100 ~ 1:150;
S2, urea and glucose joined in solution that step S1 obtains, wherein, Bi (NO 3) 35H 2the mol ratio of O and urea, glucose is 1:(2 ~ 5): (2 ~ 6);
S3, be 110 ~ 190 DEG C in reaction temperature, the reaction time is under the condition of 3 ~ 20h, and the solution that step S2 obtains carries out hydro-thermal reaction; Product is carried out separating, washing and drying, obtains described Bi 2wO 6/ C composite.
Preferably, in step S1, in described ethylene glycol and absolute ethyl alcohol mixed solution, ethylene glycol and absolute ethyl alcohol volume ratio are 1:1 ~ 1:3.
Preferably, in step S3, described hydro-thermal reaction is that the solution obtained by step S2 is transferred in hydrothermal reaction kettle, and control compactedness 40 ~ 80% is carried out.
Compared with prior art, the present invention has following beneficial effect:
The present invention prepares Bi by adopting the hydro thermal method improved 2wO 6/ C composite, C is coated on the spherical Bi of class uniformly 2wO 6on, carbon improves Bi 2wO 6conductance, can cushion Bi simultaneously 2wO 6volumetric expansion in the lithium ion battery course of work, improves stability and the cycle life of electrode.
And have compared with technology, the present invention has following beneficial effect:
1) Bi 2wO 6surface coating one deck C, effectively can improve Bi 2wO 6conductivity, improve its high rate performance in lithium ion battery, C layer can cushion Bi simultaneously 2wO 6volumetric expansion in charge and discharge process and contraction, avoid Bi 2wO 6the efflorescence of particle.
2) Bi of the present invention 2wO 6/ C has excellent high rate capability and cyclical stability and life-span.
3) method Raw of the present invention is cheaply easy to get, simple to operate, reproducible, is easy to industrialized mass production.
Accompanying drawing explanation
Fig. 1 is by the Bi prepared by embodiment 1 2wO 6/ C material SEM schemes.
Fig. 2 is by the Bi prepared by embodiment 1 2wO 6/ C material EDS schemes.
Fig. 3 is by the Bi prepared by embodiment 1 2wO 6/ C material TEM schemes.
Fig. 4 is by the Bi prepared by embodiment 1 2wO 6/ C material XRD schemes.
Fig. 5 is by the Bi prepared by embodiment 1 2wO 6the lithium ion battery multiplying power of/C material assembling and cycle performance figure.
Fig. 6 is by the Bi prepared by embodiment 2 2wO 6/ C material XRD schemes.
Fig. 7 is by the Bi prepared by embodiment 2 2wO 6the cycle performance of lithium ion battery figure of/C material assembling.
Fig. 8 is by the Bi prepared by embodiment 3 2wO 6/ C material XRD schemes.
Fig. 9 is by the Bi prepared by embodiment 3 2wO 6the cycle performance of lithium ion battery figure of/C material assembling.
Figure 10 is by the Bi prepared by comparative example 1 2wO 6/ C material SEM schemes.
Figure 11 is by the Bi prepared by comparative example 1 2wO 6the cycle performance of lithium ion battery figure of/C material assembling.
Figure 12 is by the Bi prepared by comparative example 2 2wO 6material SEM schemes.
Figure 13 is by the Bi prepared by comparative example 2 2wO 6the cycle performance of lithium ion battery figure of material assembling.
Embodiment
Below in conjunction with accompanying drawing, embodiments of the invention are elaborated: the present embodiment is implemented under premised on technical solution of the present invention, give detailed execution mode and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
Take 4.8507g (0.01mol) Bi (NO 3) 35H 2o, 1.6496g (0.005mol) Na 2wO 42H 2o joins in 55.6mL ethylene glycol and 55.6mL absolute ethyl alcohol mixed solution jointly, adds 1.2012g (0.02mol) urea while ultrasonic disperse.Take 3.6g (0.02ml) glucose directly to add in above-mentioned solution.Finally mixed liquor being loaded 100mL liner is in the hydrothermal reaction kettle of polytetrafluoroethylene, and loading is 60%.React at 150 DEG C of reaction 15h.Naturally cool to room temperature, suction filtration, washing, at 50 DEG C, dry 24h, obtains Bi 2wO 6/ C.Its pattern is as Fig. 1, and particle is that class is spherical.X-ray energy spectrum figure, as Fig. 2, can find out, material is made up of Elements C, Bi, W and O.Its high power Flied emission lens drawings, as Fig. 3, can be found out, Bi 2wO 6surface coating one deck C layer.Particle is that class is spherical.Its XRD is Fig. 4, with the contrast of standard card PDF39-0256, finds and rhombic system Bi 2wO 6base peak consistent.At 0.1-3V, under different multiplying discharge and recharge condition, Bi 2wO 6the figure of/C composite specific capacity and recurrence relation as shown in Figure 5, has good specific capacity.
Embodiment 2
Take 7.2765g (0.015mol) Bi (NO 3) 35H 2o, 2.4739g (0.0075mol) Na 2wO 42H 2o joins in 125mL ethylene glycol and 250mL absolute ethyl alcohol mixed solution jointly, adds 4.5g (0.075mol) urea while ultrasonic disperse.Take 16.2g (0.09ml) glucose directly to add in above-mentioned solution.Finally mixed liquor being loaded 100mL liner is in the hydrothermal reaction kettle of polytetrafluoroethylene, and loading is 80%.React at 190 DEG C of reaction 15h.Naturally cool to room temperature, suction filtration, washing, at 50 DEG C, dry 24h, obtains Bi 2wO 6/ C.Its XRD is Fig. 6, with the contrast of standard card PDF39-0256, finds and rhombic system Bi 2wO 6base peak consistent.Under the discharging condition of 0.1-3V, 100mA/g, Bi 2wO 6the figure of/C composite specific capacity and recurrence relation as shown in Figure 7, has good chemical property.
Embodiment 3
Take 5.8208g (0.012mol) Bi (NO 3) 35H 2o, 1.9792g (0.006mol) Na 2wO 42H 2o joins in 83.5mL ethylene glycol and 250.5mL absolute ethyl alcohol mixed solution jointly.2.852g (0.042mol) urea is added while ultrasonic disperse.Take 8.64g (0.048ml) glucose directly to add in above-mentioned solution.Finally mixed liquor being loaded 100mL liner is in the hydrothermal reaction kettle of polytetrafluoroethylene, and loading is 40%.React 110 DEG C of reaction 15h.Naturally cool to room temperature, suction filtration, washing, at 50 DEG C, dry 24h, obtains Bi 2wO 6/ C.Its XRD is Fig. 8, with the contrast of standard card PDF39-0256, finds and rhombic system Bi 2wO 6base peak consistent.Under the discharging condition of 0.1-3V, 500mA/g, Bi 2wO 6/ C composite specific capacity and recurrence relation as shown in Figure 9, have good chemical property.
Comparative example 1
Take 4.8507g (0.01mol) Bi (NO 3) 35H 2o, 1.6496g (0.005mol) Na 2wO 42H 2o joins in 55.6mL ethylene glycol and 55.6mL absolute ethyl alcohol mixed solution jointly.Get 3.6g (0.02ml) glucose while ultrasonic disperse directly to add in above-mentioned solution.Finally mixed liquor being loaded 100mL liner is in the hydrothermal reaction kettle of polytetrafluoroethylene, and loading is 60%.React at 150 DEG C of reaction 15h.Naturally cool to room temperature, suction filtration, washing, at 50 DEG C, dry 24h, obtains Bi 2wO 6/ C.Its pattern is as Figure 10.Under the discharging condition of 0.1-3V, 100mA/g, Bi 2wO 6the figure of/C composite specific capacity and recurrence relation as shown in figure 11.
Comparative example 2
Take 7.2765g (0.015mol) Bi (NO 3) 35H 2o, 2.4739g (0.0075mol) Na 2wO 42H 2o joins in 125mL ethylene glycol and 250mL absolute ethyl alcohol mixed solution jointly.4.5g (0.075mol) urea is added while ultrasonic disperse.Mixed liquor being loaded 100mL liner is in the hydrothermal reaction kettle of polytetrafluoroethylene, and loading is 80%.React at 190 DEG C of reaction 15h.Naturally cool to room temperature, suction filtration, washing, at 50 DEG C, dry 24h, obtains Bi 2wO 6.Its pattern is as Figure 12.Under the discharging condition of 0.1-3V, 100mA/g, Bi 2wO 6the figure of composite material specific capacity and recurrence relation as shown in figure 13.

Claims (4)

1. a lithium ion battery negative Bi 2wO 6/ C composite, is characterized in that, described composite material comprises the spherical Bi of class 2wO 6and be evenly coated on such spherical Bi 2wO 6outside C coating layer, described Bi 2wO 6average grain diameter be 100nm ~ 3000nm, C content is 0.5 ~ 10%.
2. a lithium ion battery negative Bi as claimed in claim 1 2wO 6the preparation method of/C composite, is characterized in that, described method comprises the steps:
S1, be the Bi (NO of 2:1 by mol ratio 3) 35H 2o and Na 2wO 42H 2o joins in the mixed solution of ethylene glycol and absolute ethyl alcohol, wherein, and Bi (NO 3) 35H 2the mol ratio of O and ethylene glycol is 1:100 ~ 1:150;
S2, urea and glucose joined in solution that step S1 obtains, wherein, Bi (NO 3) 35H 2the mol ratio of O and urea, glucose is 1:(2 ~ 5): (2 ~ 6);
S3, be 110 ~ 190 DEG C in reaction temperature, the reaction time is under the condition of 3 ~ 20h, and the solution that step S2 obtains carries out hydro-thermal reaction; Product is carried out separating, washing and drying, obtains described Bi 2wO 6/ C composite.
3. lithium ion battery negative Bi as claimed in claim 2 2wO 6the preparation method of/C composite, is characterized in that, in step S1, in described ethylene glycol and absolute ethyl alcohol mixed solution, ethylene glycol and absolute ethyl alcohol volume ratio are 1:1 ~ 1:3.
4. lithium ion battery negative Bi as claimed in claim 2 2wO 6the preparation method of/C composite, is characterized in that, in step S3, described hydro-thermal reaction is that the solution obtained by step S2 is transferred in hydrothermal reaction kettle, and control compactedness 40 ~ 80% is carried out.
CN201610077248.7A 2016-02-04 2016-02-04 A kind of high performance lithium ionic cell cathode Bi2WO6/ C composite and preparation method thereof Expired - Fee Related CN105552353B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106964339A (en) * 2017-04-14 2017-07-21 武汉理工大学 Ultra-thin Bismuth tungstate nano-sheet catalysis material of carbon doping and preparation method thereof
CN112864367A (en) * 2021-03-18 2021-05-28 贵州梅岭电源有限公司 Preparation method of lithium battery anode material with litchi-shaped sodium tungstate/nitrogen-doped carbon composite structure
CN113471420A (en) * 2021-06-23 2021-10-01 绍兴铋华科技有限公司 Bismuth tungstate coated lithium iron phosphate cathode material and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
LINSEN ZHANG ET AL: ""Synthesis and electrochemical performance of Bi2WO6/grapheme composite as anode material for lithium-ion batteries"", 《MATERIALS LETTERS》 *
刘丁菡等: "" 葡萄糖的加入量对C/Bi2WO6微晶的结构及可见光催化性能的影响"", 《人工晶体学报》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106964339A (en) * 2017-04-14 2017-07-21 武汉理工大学 Ultra-thin Bismuth tungstate nano-sheet catalysis material of carbon doping and preparation method thereof
CN106964339B (en) * 2017-04-14 2020-04-21 武汉理工大学 Carbon-doped ultrathin bismuth tungstate nanosheet photocatalytic material and preparation method thereof
CN112864367A (en) * 2021-03-18 2021-05-28 贵州梅岭电源有限公司 Preparation method of lithium battery anode material with litchi-shaped sodium tungstate/nitrogen-doped carbon composite structure
CN112864367B (en) * 2021-03-18 2022-04-19 贵州梅岭电源有限公司 Preparation method of lithium battery anode material with litchi-shaped sodium tungstate/nitrogen-doped carbon composite structure
CN113471420A (en) * 2021-06-23 2021-10-01 绍兴铋华科技有限公司 Bismuth tungstate coated lithium iron phosphate cathode material and preparation method thereof

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