CN105742608A - Mo<2>C/CNTs nanosheet electrode material and preparation method therefor - Google Patents
Mo<2>C/CNTs nanosheet electrode material and preparation method therefor Download PDFInfo
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- CN105742608A CN105742608A CN201610243164.6A CN201610243164A CN105742608A CN 105742608 A CN105742608 A CN 105742608A CN 201610243164 A CN201610243164 A CN 201610243164A CN 105742608 A CN105742608 A CN 105742608A
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- H01M10/05—Accumulators with non-aqueous electrolyte
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- 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
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- 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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a Mo<2>C/CNTs nanosheet electrode material and a preparation method therefor, and belongs to the technical field of battery materials. The preparation method comprises the following steps of 1) enabling an ammonium molybdate solution to be fully mixed with an N, N-di-n-butyl urea solution to obtain a solution A; 2) dissolving carbon nanotube CNTs into deionized water, and performing ultrasonic dispersion for 2-4h to obtain a solution B; 3) adding the solution B into the solution A in a dropwise manner, heating and evaporating the solvent until the volume of the solution is 0.01-0.1 times of the volume of the original mixed solution to obtain a turbid liquid C; 4) freezing and drying the turbid liquid C, and collecting the dried product to be used as a precursor D; and 5) performing thermal processing on the precursor D under an argon atmosphere to obtain the Mo<2>C/CNTs nanosheet electrode material. The preparation method is simple and reliable in method, free of other reducing agents, low in synthesis temperature and high in repeatability; and meanwhile, the Mo<2>C/CNTs nanosheet electrode material prepared by the method is high in crystallinity, high in purity, free of impurities, and high in electrochemical stability.
Description
Technical field
The invention belongs to battery material technical field, relate to a kind of lithium ion battery negative material preparation method,
It is specifically related to a kind of Mo2C/CNTs nanometer sheet electrode material and preparation method thereof.
Background technology
Lithium ion battery is high with its running voltage, energy density high, have extended cycle life and self discharge is little, ring
Protect the advantages such as nontoxic, in the portable electric appts such as digital camera, notebook computer and electric vehicle
Have wide application prospects.
In recent years, transition metal carbide is as a kind of Novel cathode material for lithium ion battery, by researcher
Pay close attention to.Wherein, molybdenum carbide electronic conductivity is good, good reversibility [Chen M, Zhang J, Chen Q, et al.
Construction of reduced graphene oxide supported molybdenum carbides composite
electrode as high-performance anode materials for lithium ion batteries[J].
Materials Research Bulletin, 2015,73.], it is expected to become the negative material that high rate performance is remarkable, as
Mo2C-C[Qing G,Xinyu Z,Ying X,et al.Amild route to mesoporous Mo2C–C
hybrid nanospheres for high performance lithium-ion batteries[J].Nanoscale,2014,
6 (11): 6151-6157.] at 2000mA g-1Circulate 50 circles under electric current density to remain to keep 380mAh g-1's
Charging and discharging capacity.On the other hand, molybdenum carbide can as other electric conductivity poor electrode material complex, from
And it is greatly promoted electric conductivity and the volume stability of electrode material, such as MoO2/Mo2C combination electrode exists
1000mA·g-1Circulate 140 circles under electric current density and keep 500mAh g-1Charging and discharging capacity [Zhang H J,
Wang K X,Wu X Y,et al.MoO2/Mo2C Heteronanotubes Function as
High-Performance Li-Ion Battery Electrode[J].Advanced Functional Materials,
2014,24 (22): 3,399 3404.], MoO2/Mo2C/C combination electrode is at 100mA g-1Under electric current density
Circulation 100 circle keeps 800mAh g-1Charging and discharging capacity [Mohammad Ihsan, Hongqiang Wang,
Siti R.Majid,et al.MoO2/Mo2C/C spheres as anode materials for lithium ion
Batteries [J] .Carbon, 2015,96,1200-1207.], therefore develop Mo2C-material has widely should
Use prospect.On the other hand, Mo2The synthesis technique of C is complicated, if desired at H2Reduction situation [Chen M,
Zhang J,Chen Q,et al.Construction of reduced graphene oxide supported
molybdenum carbides composite electrode as high-performance anode materials for
Lithium ion batteries [J] .Materials Research Bulletin, 2015,73.], higher synthesis temperature
(1673K)[Huang K,Bi K,Liang C,et al.Graphite Carbon-Supported Mo2C
Nanocomposites by a Single-Step Solid State Reaction for Electrochemical Oxygen
Reduction. [J] .Plos One, 2015,10 (9) .], solvent thermal-carbonization two-step synthesis method [Qing G, Xinyu Z,
Ying X,et al.A mild route to mesoporous Mo2C-C hybrid nanospheres for high
performance lithium-ion batteries.[J].Nanoscale,2014,6(11):6151-6157.].Above-mentioned system
Preparation Method condition is harsh, it is difficult to realizing industrialization and generate, thus be necessary developing low-cost, synthesis temperature is relatively
Low, the simple Mo of technique2C synthetic method is also applied to lithium ion battery negative material.
In addition, Mo2C itself is as a kind of negative material, and theoretical capacity is limited, it is therefore necessary to right
It is combined, thus promotes Mo2The actual capacity of C.
Summary of the invention
For the defect overcoming above-mentioned prior art to exist, it is an object of the invention to provide one
Mo2C/CNTs nanometer sheet electrode material and preparation method thereof, this preparation method is simple and reliable, it is not necessary to add it
Its reducing agent, and synthesis temperature is relatively low, repeatability is high；Through the Mo that the method prepares2C/CNTs nanometer sheet
Electrode material, good crystallinity, purity is high, and free from admixture has good electrical chemical stability.
The present invention is to be achieved through the following technical solutions:
The invention discloses a kind of Mo2The preparation method of C/CNTs nanometer sheet electrode material, including following step
Rapid:
1) it is 1:(0.5～2 by volume), by the ammonium molybdate solution that concentration is 1～5mol/L with concentration be
The N of 10～50mol/L, N-di-n-butyl urea liquid fully mixes, and obtains solution A；
2) CNT CNTs is dissolved in deionized water, ultrasonic disperse 2～4h, obtains solution B；
3) solution B dropwise being dropped in solution A, obtain mixed solution, heating evaporation solvent is to solution
Volume is 0.01～0.1 times of initial mixing liquor capacity, obtains suspension C；
4) by suspension C lyophilization, desciccate is collected as predecessor D；
5) by predecessor D under an argon atmosphere, in 400～700 DEG C, heat treatment 2～6h, prepare Mo2C/CNTs
Nanometer sheet electrode material.
Step 2) in the amount ratio of CNT CNTs and deionized water be (50～1000) mg:(50～80)
mL。
Step 3) it is that mixed solution is used electric heating cover, heating evaporation solvent at 50～80 DEG C.
Step 4) it is to carry out lyophilization at-50～-40 DEG C.
Step 5) control argon flow velocity be 100～300sccm.
Step 5) it is to be placed in predecessor D in square porcelain boat to carry out heat treatment.
The invention also discloses the Mo that above-mentioned employing said method prepares2C/CNTs nanometer sheet electrode material.
Compared with prior art, the present invention has a following useful technique effect:
Mo disclosed by the invention2The preparation method of C/CNTs nanometer sheet electrode material, with N, N-di-n-butyl
Reducing agent needed for carbamide offer system, becomes Mo by the reduction of ammonium molybdate one step2C nano sheet so that CNTs
Mo can be evenly affixed to2On C nano sheet.Mo2The synergism of C and CNTs, for ion and electronics
More migrating channels is provided, and can effectively prevent during ion deinsertion volumetric expansion etc., have preferably
Charge discharge capacity.The method technological process is simple and reliable, it is not necessary to adds other reducing agent, and closes
Becoming temperature relatively low (reporting 1400 DEG C of hot conditionss far below document), repeatability is high, low for equipment requirements.
Through the Mo that the inventive method prepares2C/CNTs nanometer sheet electrode material, purity is high, good crystallinity,
Adhesion is high, and free from admixture has good electrical chemical stability.
Accompanying drawing explanation
Fig. 1 is that the present invention prepares Mo2C/CNTs nanometer sheet electrode material X-ray diffractogram；
Fig. 2 is that the present invention prepares Mo2Flied emission pattern under C/CNTs nanometer sheet electrode material 50.0K multiplying power
Figure；
Fig. 3 is that the present invention prepares Mo2Flied emission pattern under C/CNTs nanometer sheet electrode material 100.0K multiplying power
Figure；
Fig. 4 is that the present invention prepares Mo2C@CNTs combination electrode material is at 100mA g-1Follow under electric current density
Ring performance map.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail, described in the present invention
Explain rather than limit.
Embodiment 1
A kind of Mo2The preparation method of C/CNTs nanometer sheet electrode material, comprises the following steps:
(1) compound concentration is 1mol/L ammonium molybdate solution 80ml, and magnetic agitation 30min makes ammonium molybdate fill
Dissolving is divided to obtain solution A standby；
(2) compound concentration is 30mol/LN, N-di-n-butyl urea liquid 40ml, magnetic agitation 20min,
Make N, N-di-n-butyl carbamide fully dissolve to obtain solution B, afterwards above-mentioned solution A be slowly added into solution B,
It is standby that mix homogeneously obtains solution C；
(3) weigh 50mg CNT to be dissolved in 80ml deionized water, ultrasonic disperse 4h, obtain molten
Liquid D is standby；
(4) above-mentioned solution D is dropwise dropped in solution C, be placed in electric jacket arranging heating-up temperature
80 DEG C, solution is gradually evaporated to the 0.05 times i.e. 10ml that liquor capacity is initial mixing liquor capacity,
To suspension E；
(5) above-mentioned suspension E is placed in culture dish, is transferred in freezer dryer, under the conditions of-40 DEG C
Lyophilization, and collect desciccate as predecessor F；
(6) above-mentioned predecessor F is transferred to square porcelain boat, is placed in argon atmosphere stove, at argon
The lower 500 DEG C of reaction 2h of gas 100sccm flow velocity, obtain Mo2C/CNTs nanometer sheet electrode material.
Embodiment 2
A kind of Mo2The preparation method of C/CNTs nanometer sheet electrode material, comprises the following steps:
(1) compound concentration is 2.5mol/L ammonium molybdate solution 60ml, and magnetic agitation 20min makes ammonium molybdate
It is standby that abundant dissolving obtains solution A；
(2) compound concentration is 30mol/LN, N-di-n-butyl urea liquid 70ml, magnetic agitation 25min,
Make N, N-di-n-butyl carbamide fully dissolve to obtain solution B, afterwards above-mentioned solution A be slowly added into solution B,
It is standby that mix homogeneously obtains solution C；
(3) weigh 150mg CNT to be dissolved in 60ml deionized water, ultrasonic disperse 3h, obtain
Solution D is standby；
(4) above-mentioned solution D is dropwise dropped in solution C, be placed in electric jacket arranging heating-up temperature
60 DEG C, solution is gradually evaporated to the 0.05 times i.e. 10ml that liquor capacity is initial mixing liquor capacity,
To suspension E；
(5) above-mentioned suspension E is placed in culture dish, is transferred in freezer dryer, under the conditions of-45 DEG C
Lyophilization, and collect desciccate as predecessor F；
(6) above-mentioned predecessor F is transferred to square porcelain boat, is placed in argon atmosphere stove, at argon
The lower 400 DEG C of reaction 5h of gas 150sccm flow velocity, obtain Mo2C/CNTs nanometer sheet electrode material.
Embodiment 3
A kind of Mo2The preparation method of C/CNTs nanometer sheet electrode material, comprises the following steps:
(1) compound concentration is 3mol/L ammonium molybdate solution 75ml, and magnetic agitation 30min makes ammonium molybdate fill
Dissolving is divided to obtain solution A standby；
(2) compound concentration is 25mol/LN, N-di-n-butyl urea liquid 70ml, magnetic agitation 15min,
Make N, N-di-n-butyl carbamide fully dissolve to obtain solution B, afterwards above-mentioned solution A be slowly added into solution B,
It is standby that mix homogeneously obtains solution C；
(3) weigh 300mg CNT to be dissolved in 80ml deionized water, ultrasonic disperse 3.5h, obtain
Solution D is standby；
(4) above-mentioned solution D is dropwise dropped in solution C, be placed in electric jacket arranging heating-up temperature
60 DEG C, solution is gradually evaporated to the 0.05 times i.e. 12ml that liquor capacity is initial mixing liquor capacity,
To suspension E；
(5) above-mentioned suspension E is placed in culture dish, is transferred in freezer dryer, under the conditions of-40 DEG C
Lyophilization, and collect desciccate as predecessor F；
(6) above-mentioned predecessor F is transferred to square porcelain boat, is placed in argon atmosphere stove, at argon
The lower 600 DEG C of reaction 3.5h of gas 250sccm flow velocity, obtain Mo2C/CNTs nanometer sheet electrode material.
Embodiment 4
A kind of Mo2The preparation method of C/CNTs nanometer sheet electrode material, comprises the following steps:
(1) compound concentration is 5mol/L ammonium molybdate solution 50ml, and magnetic agitation 25min makes ammonium molybdate fill
Dissolving is divided to obtain solution A standby；
(2) compound concentration is 40mol/LN, N-di-n-butyl urea liquid 80ml, magnetic agitation 10min,
Make N, N-di-n-butyl carbamide fully dissolve to obtain solution B, afterwards above-mentioned solution A be slowly added into solution B,
It is standby that mix homogeneously obtains solution C；
(3) weigh 800mg CNT to be dissolved in 60ml deionized water, ultrasonic disperse 2.5h, obtain
Solution D is standby；
(4) above-mentioned solution D is dropwise dropped in solution C, be placed in electric jacket arranging heating-up temperature
80 DEG C, solution is gradually evaporated to the 0.08 times i.e. 15ml that liquor capacity is initial mixing liquor capacity,
To suspension E；
(5) above-mentioned suspension E is placed in culture dish, is transferred in freezer dryer, under the conditions of-50 DEG C
Lyophilization, and collect desciccate as predecessor F；
(6) above-mentioned predecessor F is transferred to square porcelain boat, is placed in argon atmosphere stove, at argon
The lower 700 DEG C of reaction 2h of gas 300sccm flow velocity, obtain Mo2C/CNTs nanometer sheet electrode material.
See Fig. 1, prepare Mo for the present invention2C/CNTs nanometer sheet electrode material X-ray diffractogram, from
Fig. 1 is it can be seen that prepared Mo2C/CNTs nanometer sheet electrode material, for pure phase Mo2C, good crystallinity.
See Fig. 2, prepare Mo for the present invention2Flied emission pattern under C/CNTs nanometer sheet electrode material 50.0K multiplying power
Figure, figure it is seen that prepared Mo2C/CNTs nanometer sheet electrode material, CNTs is evenly affixed to
Mo2On C nano sheet, for Mo2C plays excellent support effect.
From Fig. 3 can it is further seen that, this Mo2C/CNTs nanometer sheet electrode material Mo2C nano sheet
Thickness is that 30nm, CNTs are uniformly distributed in Mo2The centre of C nano sheet and edge zone, with CNTs
It is tightly combined.Mo is reported with document2C compares, Mo prepared by the present invention2C/CNTs nanometer sheet electrode material
Material specific surface area is big, advantageously transmits in ion, it will help chemical property promotes.
Fig. 4 is this Mo2C/CNTs nanometer sheet electrode material is 100mA g in electric current density-1Time cyclicity
Can, as can be seen from Figure 4 this electrode material has higher charging and discharging capacity, from initial capacity is
3292mAh·g-1After circulating 50 times, charging and discharging capacity is gradually reduced and finally stable at 1588mAh g-1,
Showing good electrochemistry capacitance, being applied to lithium ion battery negative material has good application prospect.
Claims (7)
1. a Mo2The preparation method of C/CNTs nanometer sheet electrode material, it is characterised in that include following
Step:
1) it is 1:(0.5～2 by volume), by the ammonium molybdate solution that concentration is 1～5mol/L with concentration be
The N of 10～50mol/L, N-di-n-butyl urea liquid fully mixes, and obtains solution A；
2) CNT CNTs is dissolved in deionized water, ultrasonic disperse 2～4h, obtains solution B；
3) solution B dropwise being dropped in solution A, obtain mixed solution, heating evaporation solvent is to solution
Volume is 0.01～0.1 times of initial mixing liquor capacity, obtains suspension C；
4) by suspension C lyophilization, desciccate is collected as predecessor D；
5) by predecessor D under an argon atmosphere, in 400～700 DEG C, heat treatment 2～6h, prepare Mo2C/CNTs
Nanometer sheet electrode material.
Mo the most according to claim 12The preparation method of C/CNTs nanometer sheet electrode material, it is special
Levy and be, step 2) in the amount ratio of CNT CNTs and deionized water be (50～1000) mg:
(50～80) mL.
Mo the most according to claim 12The preparation method of C/CNTs nanometer sheet electrode material, it is special
Levy and be, step 3) it is that mixed solution is used electric heating cover, heating evaporation solvent at 50～80 DEG C.
Mo the most according to claim 12The preparation method of C/CNTs nanometer sheet electrode material, it is special
Levy and be, step 4) it is at-50～-40 DEG C, carry out lyophilization.
Mo the most according to claim 12The preparation method of C/CNTs nanometer sheet electrode material, it is special
Levy and be, step 5) to control argon flow velocity be 100～300sccm.
Mo the most according to claim 12The preparation method of C/CNTs nanometer sheet electrode material, it is special
Levy and be, step 5) it is to be placed in predecessor D in square porcelain boat to carry out heat treatment.
7. use the Mo that in claim 1～6, method described in any one prepares2C/CNTs nanometer sheet electrode
Material.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107425185A (en) * | 2017-07-17 | 2017-12-01 | 济南大学 | A kind of preparation method of carbon nanotube loaded carbonization Mo and its application in lithium sulfur battery anode material |
| CN107758668A (en) * | 2017-11-04 | 2018-03-06 | 大连理工大学 | A kind of quick method for preparing carbon load molybdenum carbide of microwave heating |
| CN109244414A (en) * | 2018-09-28 | 2019-01-18 | 陕西科技大学 | A kind of pencil MoO3@NC lithium ion battery electrode material and preparation method thereof |
| CN113394415A (en) * | 2021-06-17 | 2021-09-14 | 广西师范大学 | Oxygen-enriched vacancy NC @ BiOCl-CNTs composite material as well as preparation method and application thereof |
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| CN105217633A (en) * | 2015-09-09 | 2016-01-06 | 四川理工学院 | A kind of preparation method with the nano silicon carbide two molybdenum sheet sprills of regular hexagon structure |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107425185A (en) * | 2017-07-17 | 2017-12-01 | 济南大学 | A kind of preparation method of carbon nanotube loaded carbonization Mo and its application in lithium sulfur battery anode material |
| CN107425185B (en) * | 2017-07-17 | 2020-03-24 | 济南大学 | Preparation method of carbon nanotube-loaded molybdenum carbide material and application of carbon nanotube-loaded molybdenum carbide material in lithium-sulfur battery positive electrode material |
| CN107758668A (en) * | 2017-11-04 | 2018-03-06 | 大连理工大学 | A kind of quick method for preparing carbon load molybdenum carbide of microwave heating |
| CN109244414A (en) * | 2018-09-28 | 2019-01-18 | 陕西科技大学 | A kind of pencil MoO3@NC lithium ion battery electrode material and preparation method thereof |
| CN109244414B (en) * | 2018-09-28 | 2021-02-05 | 陕西科技大学 | Bundle-shaped MoO3@ NC lithium ion battery electrode material and preparation method thereof |
| CN113394415A (en) * | 2021-06-17 | 2021-09-14 | 广西师范大学 | Oxygen-enriched vacancy NC @ BiOCl-CNTs composite material as well as preparation method and application thereof |
| CN113394415B (en) * | 2021-06-17 | 2024-04-16 | 广西师范大学 | Oxygen-enriched vacancy NC@BiOCl-CNTs composite material and preparation method and application thereof |
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