CN105742608B - A kind of Mo2C/CNTs nanometer sheet electrode materials and preparation method thereof - Google Patents
A kind of Mo2C/CNTs nanometer sheet electrode materials and preparation method thereof Download PDFInfo
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- 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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- H01M4/58—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
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Abstract
The invention discloses a kind of Mo2C/CNTs nanometer sheet electrode materials and preparation method thereof, belong to battery material technical field, include the following steps：1) by ammonium molybdate solution and N, N di-n-butyl urea liquids mix well, and obtain solution A；2) carbon nanotube CNTs is dissolved in deionized water, 2~4h of ultrasonic disperse obtains solution B；3) solution B is added dropwise to dropwise in solution A, heating evaporation solvent to volume is originate mixeding liquid volume 0.01 0.1, obtains suspension C；4) suspension C is freeze-dried, collects desciccate as predecessor D；5) it under an argon atmosphere by predecessor D, is heat-treated, Mo is made2C/CNTs nanometer sheet electrode materials.The preparation method is simple and reliable, and without adding other reducing agents, and synthesis temperature is relatively low, and repeatability is high；Through Mo made from this method2C/CNTs nanometer sheet electrode materials, good crystallinity, purity is high, free from admixture, has good electrochemical stability.
Description
Technical field
The invention belongs to battery material technical fields, are related to a kind of lithium ion battery negative material preparation method, specifically relate to
And a kind of Mo2C/CNTs nanometer sheet electrode materials and preparation method thereof.
Background technology
Lithium ion battery is high with its operating voltage, energy density is high, have extended cycle life and self discharge is small, environment-protecting and non-poisonous etc.
Advantage has wide application prospects in the portable electronic devices such as digital camera, laptop and electric vehicle.
In recent years, transition metal carbide is paid close attention to as a kind of novel cathode material for lithium ion battery by researcher.Its
In, 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 the negative material as high rate performance brilliance, such 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.]
2000mA·g-150 circle of cycle remains to keep 380mAhg under current density-1Charging and discharging capacity.On the other hand, molybdenum carbide
The poor electrode material compound of other electric conductivity is can be used as, to greatly promote the electric conductivity and volume stability of electrode material,
Such as MoO2/Mo2C combination electrodes are in 1000mAg-1140 circle of cycle keeps 500mAhg under current density-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):3399-3404.], MoO2/Mo2C/C combination electrodes are in 100mAg-1100 circle of cycle is kept under current density
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 Mo is developed2C-material is with a wide range of applications.On the other hand, Mo2The synthesis technology of C
Complexity is such as needed in H2The case where reduction [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
Heat-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 preparation method condition is harsh, it is difficult to realize that industrialization generates, because
And it is necessary to developing low-cost, synthesis temperature is relatively low, Mo simple for process2C synthetic methods are simultaneously applied to negative electrode of lithium ion battery
Material.
In addition to this, Mo2C itself is used as a kind of negative material, theoretical capacity limited, it is therefore necessary to and it is compound to its, from
And promote Mo2The actual capacity of C.
Invention content
In order to overcome the problems of the above-mentioned prior art, the purpose of the present invention is to provide a kind of Mo2C/CNTs nanometers
Plate electrode material and preparation method thereof, the preparation method is simple and reliable, and without adding other reducing agents, and synthesis temperature is relatively low,
It is repeated high；Through Mo made from this method2C/CNTs nanometer sheet electrode materials, good crystallinity, purity is high, free from admixture, has good
Good electrochemical 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 materials, includes the following steps：
1) it is 1 by volume:(0.5~2), by the ammonium molybdate solution of a concentration of 1~5mol/L with a concentration of 10~
The N of 50mol/L, N- di-n-butyl urea liquid mix well, and obtain solution A；
2) carbon nanotube CNTs is dissolved in deionized water, 2~4h of ultrasonic disperse obtains solution B；
3) solution B is added dropwise to dropwise in solution A, obtains mixed solution, heating evaporation solvent to liquor capacity is initial
0.01~0.1 times of mixed liquor volume, obtains suspension C；
4) suspension C is freeze-dried, collects desciccate as predecessor D；
5) under an argon atmosphere by predecessor D, in 400~700 DEG C, it is heat-treated 2~6h, Mo is made2C/CNTs nanometer sheets
Electrode material.
Carbon nanotube CNTs and the amount ratio of deionized water are (50~1000) mg in step 2)：(50~80) mL.
Step 3) is that mixed solution is used electric heating cover, the heating evaporation solvent at 50~80 DEG C.
Step 4) is freeze-dried at -50~-40 DEG C.
It is 100~300sccm that step 5), which controls argon gas flow velocity,.
Step 5) is that predecessor D is placed in rectangular porcelain boat to be heat-treated.
The invention also discloses above-mentioned using Mo made from the above method2C/CNTs nanometer sheet electrode materials.
Compared with prior art, the present invention has technique effect beneficial below：
Mo disclosed by the invention2The preparation method of C/CNTs nanometer sheet electrode materials, with N, N- di-n-butyl urea provides
The reduction of one step of ammonium molybdate is become Mo by reducing agent needed for system2C nano piece so that CNTs can be evenly affixed to Mo2C nano
On piece.Mo2The synergistic effect of C and CNTs provides more migrating channels for ion and electronics, and it is de- effectively to prevent ion
Volume expansion etc. during embedding, has preferable charge discharge capacity.This method technological process is simple and reliable, without addition
Other reducing agents, and synthesis temperature is relatively low (being far below 1400 DEG C of hot conditions of document report), repeatability is high, to equipment requirement
It is low.
Through Mo made from the method for the present invention2C/CNTs nanometer sheet electrode materials, purity is high, good crystallinity, and binding force is high, nothing
Impurity has good electrochemical stability.
Description of the drawings
Fig. 1 is that the present invention prepares Mo2C/CNTs nanometer sheet electrode material X-ray diffractograms；
Fig. 2 is that the present invention prepares Mo2Flied emission shape appearance figure under C/CNTs nanometer sheet electrode material 50.0K multiplying powers；
Fig. 3 is that the present invention prepares Mo2Flied emission shape appearance figure under C/CNTs nanometer sheet electrode material 100.0K multiplying powers；
Fig. 4 is that the present invention prepares Mo2C@CNTs combination electrode materials are in 100mAg-1Cycle performance figure under current density.
Specific implementation mode
With reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and
It is not to limit.
Embodiment 1
A kind of Mo2The preparation method of C/CNTs nanometer sheet electrode materials, includes the following steps：
(1) compound concentration is 1mol/L ammonium molybdate solution 80ml, magnetic agitation 30min, so that ammonium molybdate is fully dissolved and obtains
Solution A is spare；
(2) compound concentration is 30mol/LN, and N- di-n-butyls urea liquid 40ml, magnetic agitation 20min make N, N- bis- is just
Butyl urea fully dissolves to obtain solution B, and above-mentioned solution A is slowly added into solution B later, uniformly mixed that solution C is spare；
(3) it weighs 50mg carbon nanotubes to be dissolved in 80ml deionized waters, it is spare to obtain solution D by ultrasonic disperse 4h；
(4) above-mentioned solution D is added dropwise in solution C dropwise, is placed in 80 DEG C of heating temperature of setting in electric jacket, it will be molten
Liquid is gradually evaporated to the 0.05 times i.e. 10ml that liquor capacity is initial mixing liquor capacity, obtains suspension E；
(5) above-mentioned suspension E is placed in culture dish, is transferred in freeze drier, is freeze-dried under the conditions of -40 DEG C,
And desciccate is collected as predecessor F；
(6) above-mentioned predecessor F is transferred to rectangular porcelain boat, be placed in argon atmosphere stove, flowed in argon gas 100sccm
The lower 500 DEG C of reactions 2h of speed, obtains Mo2C/CNTs nanometer sheet electrode materials.
Embodiment 2
A kind of Mo2The preparation method of C/CNTs nanometer sheet electrode materials, includes the following steps：
(1) compound concentration, which is 2.5mol/L ammonium molybdate solution 60ml, magnetic agitation 20min, makes ammonium molybdate fully dissolve
It is spare to solution A；
(2) compound concentration is 30mol/LN, and N- di-n-butyls urea liquid 70ml, magnetic agitation 25min make N, N- bis- is just
Butyl urea fully dissolves to obtain solution B, and above-mentioned solution A is slowly added into solution B later, uniformly mixed that solution C is spare；
(3) it weighs 150mg carbon nanotubes to be dissolved in 60ml deionized waters, it is spare to obtain solution D by ultrasonic disperse 3h；
(4) above-mentioned solution D is added dropwise in solution C dropwise, is placed in 60 DEG C of heating temperature of setting in electric jacket, it will be molten
Liquid is gradually evaporated to the 0.05 times i.e. 10ml that liquor capacity is initial mixing liquor capacity, obtains suspension E；
(5) above-mentioned suspension E is placed in culture dish, is transferred in freeze drier, is freeze-dried under the conditions of -45 DEG C,
And desciccate is collected as predecessor F；
(6) above-mentioned predecessor F is transferred to rectangular porcelain boat, be placed in argon atmosphere stove, flowed in argon gas 150sccm
The lower 400 DEG C of reactions 5h of speed, obtains Mo2C/CNTs nanometer sheet electrode materials.
Embodiment 3
A kind of Mo2The preparation method of C/CNTs nanometer sheet electrode materials, includes the following steps：
(1) compound concentration is 3mol/L ammonium molybdate solution 75ml, magnetic agitation 30min, so that ammonium molybdate is fully dissolved and obtains
Solution A is spare；
(2) compound concentration is 25mol/LN, and N- di-n-butyls urea liquid 70ml, magnetic agitation 15min make N, N- bis- is just
Butyl urea fully dissolves to obtain solution B, and above-mentioned solution A is slowly added into solution B later, uniformly mixed that solution C is spare；
(3) it weighs 300mg carbon nanotubes to be dissolved in 80ml deionized waters, it is spare to obtain solution D by ultrasonic disperse 3.5h；
(4) above-mentioned solution D is added dropwise in solution C dropwise, is placed in 60 DEG C of heating temperature of setting in electric jacket, it will be molten
Liquid is gradually evaporated to the 0.05 times i.e. 12ml that liquor capacity is initial mixing liquor capacity, obtains suspension E；
(5) above-mentioned suspension E is placed in culture dish, is transferred in freeze drier, is freeze-dried under the conditions of -40 DEG C,
And desciccate is collected as predecessor F；
(6) above-mentioned predecessor F is transferred to rectangular porcelain boat, be placed in argon atmosphere stove, flowed in argon gas 250sccm
The lower 600 DEG C of reactions 3.5h of speed, obtains Mo2C/CNTs nanometer sheet electrode materials.
Embodiment 4
A kind of Mo2The preparation method of C/CNTs nanometer sheet electrode materials, includes the following steps：
(1) compound concentration is 5mol/L ammonium molybdate solution 50ml, magnetic agitation 25min, so that ammonium molybdate is fully dissolved and obtains
Solution A is spare；
(2) compound concentration is 40mol/LN, and N- di-n-butyls urea liquid 80ml, magnetic agitation 10min make N, N- bis- is just
Butyl urea fully dissolves to obtain solution B, and above-mentioned solution A is slowly added into solution B later, uniformly mixed that solution C is spare；
(3) it weighs 800mg carbon nanotubes to be dissolved in 60ml deionized waters, it is spare to obtain solution D by ultrasonic disperse 2.5h；
(4) above-mentioned solution D is added dropwise in solution C dropwise, is placed in 80 DEG C of heating temperature of setting in electric jacket, it will be molten
Liquid is gradually evaporated to the 0.08 times i.e. 15ml that liquor capacity is initial mixing liquor capacity, obtains suspension E；
(5) above-mentioned suspension E is placed in culture dish, is transferred in freeze drier, is freeze-dried under the conditions of -50 DEG C,
And desciccate is collected as predecessor F；
(6) above-mentioned predecessor F is transferred to rectangular porcelain boat, be placed in argon atmosphere stove, flowed in argon gas 300sccm
The lower 700 DEG C of reactions 2h of speed, obtains Mo2C/CNTs nanometer sheet electrode materials.
Referring to Fig. 1, Mo is prepared for the present invention2C/CNTs nanometer sheet electrode material X-ray diffractograms, it will be seen from figure 1 that
Prepared Mo2C/CNTs nanometer sheet electrode materials are pure phase Mo2C, good crystallinity.Referring to Fig. 2, Mo is prepared for the present invention2C/
Flied emission shape appearance figure under CNTs nanometer sheet electrode material 50.0K multiplying powers, figure it is seen that prepared Mo2C/CNTs nanometer sheets
Electrode material, CNTs are evenly affixed to Mo2C nano on piece is Mo2C plays the role of excellent support.
From Fig. 3 can with it is further seen that, the Mo2C/CNTs nanometer sheet electrode materials Mo2C nano piece thickness is 30nm,
CNTs is uniformly distributed in Mo2The centre and edge zone of C nano piece, are tightly combined with CNTs.With document report Mo2C is compared,
Mo prepared by the present invention2C/CNTs nanometer sheet electrode material large specific surface areas are more conducive to ion transmission, it will help electrification
Learn performance boost.
Fig. 4 is the Mo2C/CNTs nanometer sheets electrode material is 100mAg in current density-1When cycle performance, from Fig. 4
It can be seen that the electrode material has higher charging and discharging capacity, it is 3292mAhg from initial capacity-1After cycle 50 times,
Charging and discharging capacity is gradually reduced and finally stablizes in 1588mAhg-1, show good electrochemistry capacitance, be applied to lithium from
Sub- cell negative electrode material has good application prospect.
Claims (5)
1. a kind of Mo2The preparation method of C/CNTs nanometer sheet electrode materials, which is characterized in that include the following steps：
1) it is 1 by volume:(0.5~2), by the ammonium molybdate solution of a concentration of 1~5mol/L with a concentration of 10~50mol/L's
N, N- di-n-butyl urea liquid mix well, and obtain solution A；
2) carbon nanotube CNTs is dissolved in deionized water, 2~4h of ultrasonic disperse obtains solution B；It carbon nanotube CNTs and goes
The amount ratio of ionized water is (50~1000) mg：(50~80) mL；
3) solution B is added dropwise to dropwise in solution A, obtains mixed solution, mixed solution is used into electric heating cover, at 50~80 DEG C
Lower heating evaporation solvent obtains suspension C to 0.01~0.1 times that liquor capacity is initial mixing liquor capacity；
4) suspension C is freeze-dried, collects desciccate as predecessor D；
5) under an argon atmosphere by predecessor D, in 400~700 DEG C, it is heat-treated 2~6h, Mo is made2C/CNTs nanometers of plate electrode materials
Material.
2. Mo according to claim 12The preparation method of C/CNTs nanometer sheet electrode materials, which is characterized in that step 4) is
It is freeze-dried at -50~-40 DEG C.
3. Mo according to claim 12The preparation method of C/CNTs nanometer sheet electrode materials, which is characterized in that step 5) is controlled
Argon gas flow velocity processed is 100~300sccm.
4. Mo according to claim 12The preparation method of C/CNTs nanometer sheet electrode materials, which is characterized in that step 5) is
Predecessor D is placed in rectangular porcelain boat and is heat-treated.
5. using Mo made from any one of Claims 1 to 4 the method2C/CNTs nanometer sheet electrode materials.
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| CN107758668B (en) * | 2017-11-04 | 2020-09-29 | 大连理工大学 | Method for rapidly preparing carbon-loaded molybdenum carbide through microwave heating |
| 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 |
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