CN109449398A - A kind of preparation method and applications of lithium ion battery conductive agent nitrogen-doped graphene - Google Patents

A kind of preparation method and applications of lithium ion battery conductive agent nitrogen-doped graphene Download PDF

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Publication number
CN109449398A
CN109449398A CN201811235110.0A CN201811235110A CN109449398A CN 109449398 A CN109449398 A CN 109449398A CN 201811235110 A CN201811235110 A CN 201811235110A CN 109449398 A CN109449398 A CN 109449398A
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China
Prior art keywords
nitrogen
conductive agent
graphene
lithium ion
ion battery
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CN201811235110.0A
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Inventor
葛昊
修忠海
朱帅
孙智佳
郭欣
张诏
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Liaoning University
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Liaoning University
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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
    • H01M4/62—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
    • 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
    • H01M4/364—Composites as mixtures
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The present invention provides a kind of preparation method and applications of lithium ion battery conductive agent nitrogen-doped graphene, belong to technical field of lithium batteries.Specifically the preparation method comprises the following steps: 1) at room temperature, graphene is placed in distilled water after ultrasound, nitrogen source is added and is placed at room temperature for 10-14h, 50 DEG C of vacuum drying 12h；2) above-mentioned product is placed in tube furnace argon atmosphere, 600 DEG C of calcining 1h；3) activator is added in Xiang Shangshu product to be placed under tube furnace argon atmosphere and calcine after grinding under infrared lamp, cooled to room temperature, distillation water washing centrifugation, 50 DEG C of vacuum drying 12h, grinding obtains target product.Lithium ion battery conductive agent nitrogen-doped graphene material, one side safety and environmental protection can solve the security hidden trouble of lithium battery material, and the electronegativity of material can be improved in the incorporation of another aspect nitrogen-atoms, to improve the chemical property of material.

Description

A kind of preparation method and applications of lithium ion battery conductive agent nitrogen-doped graphene
Technical field
The present invention relates to technical field of lithium ion, specifically provide a kind of lithium ion battery conductive agent N doping graphite The preparation method and applications of alkene.
Background technique
Lithium ion battery becomes current electronic because having many advantages, such as that specific capacity is high, cycle life is high, at low cost, high magnification One of automobile preferred power units.The unnecessary addition conductive agent of lithium ion battery improves electric conductivity in principle, but for power Type lithium ion battery, a little conductive agent, which is added, can improve contact resistance between negative electrode active material, make leading for each position of electrode It is electrically consistent, so that the performance of battery is preferably played when high current charge-discharge.The addition of conductive agent can be in active material Between, between active material and collector collect micro-current, to reduce the contact resistance of electrode, accelerate the rate travel of electronics, Migration rate of the lithium ion in electrode material can be also effectively improved simultaneously, to improve the efficiency for charge-discharge of electrode.
Different types of conductive agent has different property and shape.Common conductive agent can be divided into granular conductive agent, Such as acetylene black, conductive black (SP)；Fibrous conductive agent, such as carbon nanotube (CNT), carbon fiber (VGCF).Acetylene black is because of crystalline substance Degree of formatting is low, lithium ion is embedded in is not much different with abjection Gibbs free energy wherein；And acetylene black conductivity is larger, resistance Heat release is small, therefore security performance is high, therefore is widely used among lithium ion battery conductive agent.Conductive black and graphite have fine Electric conductivity, density is small, stable structure and chemical stability, be commonly used for the conductive agent of anode material for lithium-ion batteries.Carbon is received Mitron has crystallinity high, and there are the big pi bonds of delocalization for tube wall, and it is with fibrous structure, is conducive to be formed in the electrodes effectively Conductive network and fixed electrode material.
In recent years, those skilled in the relevant arts' research is prepared for different conductive agent materials, and achieves certain achievement. Thorat etc. uses LiFePO4As active material, when being mixed with carbonaceous conductive agent carbon fiber and carbon black, discovery positive electrode has very High volumetric properties.
Lin etc. makees conductive agent with regard to carbon nanotube (CNT) and carbon black (CB) respectively, studies it to LiFePO4/ graphite cell It influences.Research finds that the battery for making conductive agent composition with carbon nanotube, carbon black all reaches 113mAh/ in 0.1C multiplying power discharge capacity G, and the battery that conductive agent CNT ratio CB is added under 1C multiplying power has higher capacity.CNT conductive agent battery, and 0.1C multiplying power is followed After ring 50 times, capacity still retains 99.2%；Polarizing voltage 0.3V drops to 0.2V, and impedance is decreased obviously.
Li et al., respectively as conductive agent, studies it to LiFePO with regard to carbon nanotube and acetylene black4The influence of performance, will LiFePO4: PVDF: conductive agent mass ratio is that 9:1:1 forms battery.The initial capacity 155mAh/g in 0.1C multiplying power discharging, is followed Ring efficiency is 95%, still reaches 122mAh/g in 5C rate capability.Carbon nanotube conducting agent improves electronics in LiFePO4It is connect with electric current Transfer on tentaculum interface, to improve chemical property, it is seen that for the lithium ion battery for developing high capacity, carbon nanotube conduct New conductive agent has very big potentiality.
Graphene is introduced lithium titanate anode by Zhang etc., and discusses in detail to conductivity threshold problem. When graphene dosage is 5%, the chemical property of lithium titanate is higher than the performance using 15% carbon black.Using grain spacing from general It reads, show that the conductivity threshold of graphene is 0.54% by simulating, 1 order of magnitude lower than carbon black shows stone from quantitative angle Black alkene conductive agent has good conductive effect.
Piao etc. uses KOH activation method, hole abundant is introduced on the surface of graphene, then as the conduction of LFP Agent uses activated graphene significantly to be promoted as the LFP high rate performance of conductive agent, and LFP capacity still has when current density 5A/g 60mAh/g or more.
This further illustrates graphene sheet layers to have influence to lithium ion transport in LFP system, while being also graphite The practical application of alkene conductive agent provides a kind of new thinking.Currently, conductive agent is studied, domestic and international scientific research personnel is had been achieved for And industrial circle is more and more paid close attention to.Therefore, a kind of efficient lithium ion battery conductive agent nitrogen-doped graphene material is explored to compel The eyebrows and eyelashes.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of lithium ion battery conductive agent nitrogen-doped graphene and its answer With to improve contact resistance between lithium ion battery negative material, to make battery performance play more in high current charge-discharge It is good.
Technical solution provided by the invention, a kind of preparation method of lithium ion battery conductive agent nitrogen-doped graphene, including Following steps:
1) at room temperature, graphene is placed in distilled water after ultrasound 15-30min, nitrogen source is added and is placed at room temperature for 10-14h, 50 DEG C vacuum drying；
2) step 1) products therefrom is placed in tube furnace, under argon atmosphere, 600 DEG C of calcining 1h obtain nitrogen source/graphite Alkene combination product；
3) activator is added into nitrogen source/graphene combination product to be placed in tube furnace, after grinding under infrared lamp in argon Atmosphere encloses lower calcining, and cooled to room temperature distills water washing, centrifugation, and 50 DEG C of obtained solid object vacuum drying are regrind, Obtain target product.
Preferably, a kind of preparation method of above-mentioned lithium ion battery conductive agent nitrogen-doped graphene, the nitrogen source are Silk, the activator are KOH.
It is furthermore preferred that a kind of preparation method of above-mentioned lithium ion battery conductive agent nitrogen-doped graphene, in mass ratio, stone Black alkene: silk=1:1-5.
It is furthermore preferred that a kind of preparation method of above-mentioned lithium ion battery conductive agent nitrogen-doped graphene, in mass ratio, step It is rapid 3) in the ratio between KOH and silk/graphene combination product be 1:1-5.
Preferably, the preparation method of above-mentioned a kind of lithium ion battery conductive agent nitrogen-doped graphene, step 3) calcining temperature 400-700 DEG C of degree.
Preferably, the preparation method of above-mentioned a kind of lithium ion battery conductive agent nitrogen-doped graphene, when step 3) is calcined Between be 1-3h.
Application of the nitrogen-doped graphene prepared according to above-mentioned method as conductive agent in lithium ion battery.Method is such as Under: negative electrode material, binder and conductive agent are stirred evenly coated on the cathode on copper foil as lithium ion battery；Described leads Electric agent is nitrogen-doped graphene prepared by above-mentioned method.
Preferably, the negative electrode material is Li4Ti5O12, binder is PVDF (Kynoar).
Preferably, by weight, Li4Ti5O12: PVDF: nitrogen-doped graphene=7-8:1:1-2.
The beneficial effects of the present invention are:
1. the present invention is using natural silk and graphene as raw material, using distilled water as solvent, in impregnating under room temperature, and vacuum Dry, high-temperature calcination obtains silk/graphene combination product；Using KOH as activator, nitrogen-doped graphene material is prepared, is closed It is easy to control at process condition, it is easy to operate, it is easy to industrialized production.
2. the present invention is using natural silk as nitrogen source, environmentally protective and nitrogen content is high, the nitrogen-doped graphene material prepared Material, large specific surface area, and the contact resistance of electrode can be reduced, accelerate the rate travel of electronics, while can also effectively improve Migration rate of the lithium ion in electrode material, to improve the efficiency for charge-discharge of electrode.
3. the present invention uses natural silk for raw material, the nitrogen-doped graphene material of preparation is easy to get with raw material, It is environmentally protective, it is sustainable the features such as, and the material prepared has the characteristics that nitrogen content is higher high with degree of graphitization.The present invention Nitrogen-doped graphene introduces silk in graphene film interlayer, and the incorporation of nitrogen-atoms changes the electronegativity of C atom, and increasing can inhale The active site of electronics needed for attached more reactions increases counterfeit electricity so that electrode material surface is easy to happen redox reaction Hold, the chemical property of material significantly improves.
Detailed description of the invention
Fig. 1 is the XRD diagram of graphene (a), nitrogen-doped graphene (b).
Fig. 2 is the Raman figure of graphene (b), nitrogen-doped graphene (a).
Fig. 3 is the SEM figure of graphene (a), nitrogen-doped graphene (b).
Specific embodiment
The guarantor that the present invention is further explained, but is not intended to restrict the invention below with reference to specific embodiment Protect range.
In order to improve lithium ion battery chemical property, the suitable alternative of conductive agent acetylene black is found, the present invention provides A kind of preparation and its application of lithium ion battery conductive agent nitrogen-doped graphene, include the following steps:
1) at room temperature, graphene is placed in distilled water after ultrasound 15-30min, silk is added, is placed at room temperature for 10-14h, 50 DEG C of vacuum drying 12h；
2) above-mentioned products therefrom is placed in tube furnace, under argon atmosphere, 600 DEG C of calcining 1h obtain silk/graphene Combination product；
3) certain mass KOH is added into silk/graphene combination product to be placed in tube furnace after grinding under infrared lamp, Under argon atmosphere, 400-700 DEG C of calcining 1-3h, cooled to room temperature distills water washing, is centrifuged, 50 DEG C of obtained solid object Vacuum drying, grinding, obtains target product.
Wherein, graphene is ultrasonically treated with distilled water, is to be dispersed in graphene uniform in distilled water.By silk Room temperature is steeped in graphene dispersion solution, is to mix graphene uniformly with silk.First time tube furnace high-temperature calcination is In order to make Filamentous silk, it is sintered into powder, and preferably mix with graphene.It is ground for the second time with KOH, tube furnace high temperature Calcining is using KOH as activator, to prepare nitrogen-doped graphene conduction agent material.
In order to prepare better nitrogen-doped graphene conduction agent material, the chemical property of lithium ion battery is improved, it is preferable that KOH is ground with silk/graphene combination product according to mass ratio 1:1-5.
1 lithium ion battery conductive agent nitrogen-doped graphene of embodiment
(1) it prepares
1) at room temperature, 0.05g graphene is placed in 10mL distilled water, after ultrasonic 30min, 0.25g silk, room temperature is added Place 12h, 50 DEG C of vacuum drying 12h；
2) above-mentioned products therefrom is placed in tube furnace, under argon atmosphere, 600 DEG C of calcining 1h obtain silk/graphene Combination product；
3) 0.8g KOH is added into 0.2g silk/graphene combination product and is placed in tube furnace after grinding under infrared lamp In, under argon atmosphere, 800 DEG C of calcining 4h, cooled to room temperature, distillation water washing centrifugation 5 times, 50 DEG C of vacuum drying 12h, Regrinding, obtains target product.
(2) it detects
Nitrogen-doped graphene prepared in graphene and embodiment 1 (one) is subjected to XRD, Raman and SEM electron-microscope scanning Detection, as a result as shown in Figure 1, Figure 2, Figure 3 shows.
(a) is graphene XRD diagram in Fig. 1, and (b) is nitrogen-doped graphene XRD diagram in Fig. 1.(a) is at 2 θ=11 ° in Fig. 1 There is a spike, be the characteristic peak of graphene, 2 θ=27 ° (b) are there are a broad peak in Fig. 1, and (b) is compared with peak (a) in Fig. 1 in Fig. 1 Value movement, and peak width broadens, it was demonstrated that N element is successfully entrained in material nitrogen-doped graphene.
(a) is nitrogen-doped graphene raman spectrum in Fig. 2, and (b) is graphite Raman spectrogram in Fig. 2.It can be seen that graphite Alkene is in 1394cm-1、1594cm-1There are the peaks D and the peak G, and nitrogen-doped graphene is in 1344cm-1、1584cm-1Place there are the peak D and the peak G, And the peak D and G peak intensity ratio (ID/ IG) graphene is 0.88, nitrogen-doped graphene 1, ID/IGIllustrate greatly in material rich in N member Element.
(a) is that the SEM of graphene schemes in Fig. 3, and (b) is that the SEM of nitrogen-doped graphene schemes in Fig. 3.It can be seen in Fig. 3 Out, graphene is many laminated structures of fold, and the amount of crimp of laminated structure is fairly obvious in nitrogen-doped graphene.
Complex chart 1, Fig. 2, Fig. 3 can be obtained, and 1 gained nitrogen-doped graphene material of embodiment, is apparent with amount of crimp Material, and doped with N element.
2 nitrogen-doped graphene of embodiment is as the application in lithium ion battery conductive agent
(1) assembly of lithium ion battery
1) market is taken to buy common Li4Ti5O12(LTO) made as binder, embodiment 1 as negative electrode material, PVDF Standby nitrogen-doped graphene is as conductive agent, and in mass ratio, 8:1:1 carries out mixing mixing paste, is evenly applied on copper foil as negative Pole is assembled into button cell using lithium piece as anode.
2) market is taken to buy common Li4Ti5O12(LTO) made as binder, embodiment 1 as negative electrode material, PVDF Standby nitrogen-doped graphene is as conductive agent, and in mass ratio, 7.8:1:1.2 carries out mixing mixing paste, is evenly applied to make on copper foil Button cell is assembled into using lithium piece as anode for cathode.
3) market is taken to buy common Li4Ti5O12(LTO) made as binder, embodiment 1 as negative electrode material, PVDF Standby nitrogen-doped graphene is as conductive agent, and in mass ratio, 7.9:1:1.1 carries out mixing mixing paste, is evenly applied to make on copper foil Button cell is assembled into using lithium piece as anode for cathode.
Comparative example 1
Market is taken to buy common Li4Ti5O12(LTO) it is used as negative electrode material, PVDF as binder, acetylene black conductive Agent, in mass ratio, 8:1:1 carry out mixing mixing paste, are evenly applied on copper foil, using lithium piece as anode, be assembled into as cathode Button cell.
(2) electrochemical property test
Button cell prepared by different conductive agents is subjected to electro-chemical test, the results are shown in Table 1.
The chemical property of battery prepared by the different conductive agents of table 1 compares (charge-discharge magnification 1C)
Seen from table 1, compared to acetylene black conductor, the electricity of the nitrogen-doped graphene conductive agent of method synthesis of the invention Chemical property is improved significantly, and with the increase of nitrogen-doped graphene, conductive agent material synthesized by the method for the present invention Chemical property first improves to be weakened afterwards, and can be seen that negative electrode material, PVDF, nitrogen-doped graphene mass ratio are 7.9:1:1.1 Prepared battery material, chemical property are obviously significantly larger than obtained material under other conditions, are keeping conductive agent Under the premise of good characteristic, the safety problem of lithium battery, and the doping of nitrogen-atoms are not only solved, the electrification of material is improved Learn performance, and raw material use natural silk, it is environmentally protective, be easy to get, provide a kind of higher lithium of chemical property from The conductive agent of sub- battery.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.

Claims (10)

1. a kind of preparation method of lithium ion battery conductive agent nitrogen-doped graphene, which comprises the steps of:
1) at room temperature, graphene is placed in distilled water after ultrasound 15-30min, nitrogen source is added, is placed at room temperature for 10-14h, 50 DEG C Vacuum drying；
2) step 1) products therefrom is placed in tube furnace, under argon atmosphere, it is multiple to obtain nitrogen source/graphene by 600 DEG C of calcining 1h Close product；
3) activator is added into nitrogen source/graphene combination product to be placed in tube furnace, after grinding under infrared lamp in argon atmospher Lower calcining is enclosed, cooled to room temperature distills water washing, centrifugation, and 50 DEG C of obtained solid object vacuum drying regrind, obtain mesh Mark product.
2. a kind of preparation method of lithium ion battery conductive agent nitrogen-doped graphene described in accordance with the claim 1, feature exist In the nitrogen source is silk, and the activator is KOH.
3. a kind of preparation method of lithium ion battery conductive agent nitrogen-doped graphene, feature exist according to claim 2 In, in mass ratio, graphene: silk=1:1-5.
4. a kind of preparation method of lithium ion battery conductive agent nitrogen-doped graphene, feature exist according to claim 2 In in mass ratio, the ratio between KOH and silk/graphene combination product are 1:1-5 in step 3).
5. a kind of preparation method of lithium ion battery conductive agent nitrogen-doped graphene described in accordance with the claim 1, feature exist In 400-700 DEG C of step 3) calcination temperature.
6. a kind of preparation method of lithium ion battery conductive agent nitrogen-doped graphene described in accordance with the claim 1, feature exist In step 3) calcination time is 1-3h.
7. according to the nitrogen-doped graphene of method described in any one of claims 1-6 preparation as conductive agent in lithium ion battery In application.
8. applying according to claim 7, which is characterized in that method is as follows: negative electrode material, binder and conductive agent are stirred Even application is mixed in the cathode on copper foil as lithium ion battery；The conductive agent is described in any one of claims 1-6 The nitrogen-doped graphene of method preparation.
9. applying according to claim 8, which is characterized in that the negative electrode material is Li4Ti5O12, binder is PVDF。
10. applying according to claim 9, which is characterized in that by weight, Li4Ti5O12: PVDF: nitrogen-doped graphene =7-8:1:1-2.
CN201811235110.0A 2018-10-23 2018-10-23 A kind of preparation method and applications of lithium ion battery conductive agent nitrogen-doped graphene Pending CN109449398A (en)

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Cited By (1)

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CN115000389A (en) * 2022-07-15 2022-09-02 湖北亿纬动力有限公司 Negative electrode material and preparation method and application thereof
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Application publication date: 20190308