CN108183203A - The preparation method of multilevel hierarchy molybdenum carbide/nitrogen-doped carbon complex microsphere electrode material - Google Patents
The preparation method of multilevel hierarchy molybdenum carbide/nitrogen-doped carbon complex microsphere electrode material Download PDFInfo
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- CN108183203A CN108183203A CN201711265228.3A CN201711265228A CN108183203A CN 108183203 A CN108183203 A CN 108183203A CN 201711265228 A CN201711265228 A CN 201711265228A CN 108183203 A CN108183203 A CN 108183203A
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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
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- 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 relates to a kind of preparation methods of multilevel hierarchy molybdenum carbide/nitrogen-doped carbon complex microsphere electrode material, include the following steps：S1. copper acetate, L glutamic acid and phosphomolybdic acid are descended into stirring and dissolving in the water of 30 60 DEG C of temperature；S2. by stirring and dissolving lower in the water of 30 60 DEG C of temperature of melamine；S3. the solution in above-mentioned above-mentioned steps S1 and S2 is mixed, is stirred to react 12 72h at being 50 90 DEG C in temperature, then filters and wash filter cake with ethyl alcohol, in 50 DEG C of vacuum drying for 24 hours, obtain presoma；S4. above-mentioned precursor is heated to 500 800 DEG C in an inert atmosphere, is slowly cooled to room temperature after 1 5h of isothermal holding, products therefrom is in FeCl360 DEG C of solution stirring 6h, filter and use the filtered filter cake of pure water, be dried in vacuo filter cake for 24 hours at a temperature of 80 DEG C.Beneficial effects of the present invention：With higher specific capacity, good cycle performance and high rate performance, simple for process, cost of material is low, is easy to industrial scale production.
Description
Technical field
The present invention relates to lithium ion battery electrode material technology of preparing, it particularly relates to a kind of multilevel hierarchy molybdenum carbide/
The preparation method of nitrogen-doped carbon complex microsphere electrode material.
Background technology
As currently commercially most widely used lithium ion battery negative material, the actual specific capacity of graphite is very
Close to its theoretical capacity 372mAhg-1.As market is to the growing of high-performance lithium battery requirements, seek novel high-capacity
Negative material is particularly important.Because have many advantages, such as good electron conduction, steady chemical structure and, molybdenum carbide（MoC）Quilt
For showing good chemical property during lithium ion battery negative material, reversible capacity can reach the 2- of graphite cathode
3 times.However, in order to ensure that materials serve goes out higher storage lithium activity, molybdenum carbide needs to be prepared to several nanometers to tens of grain size
The particle shape of nanometer.Due to the characteristic of nano material high-ratio surface energy itself, molybdenum carbide particles are in conventional high-temperature preparation process
High temperature agglomeration can inevitably occur, so as to seriously reduce the electro-chemical activity of molybdenum carbide cathode.
To overcome the above problem existing for traditional preparation process, people study and propose gas phase thermal reduction.Passing through will
Molybdenum oxygen compound is supported in carbon skeleton matrix, and carbothermic reduction reaction occurs with organic carbon small molecule under the high temperature conditions, real
The uniform distribution of nanoscale molybdenum carbide particles is showed.
Molybdenum carbide nano particle can effectively promote the chemical property of electrode material with carbon-based bluk recombination.On the one hand, carbon
Place of the skeleton matrix as carbothermic reduction reaction itself can play the role of inhibiting nanoparticle agglomerates under high temperature.It is another
Aspect, carbon skeleton matrix also avoid being in direct contact for molybdenum carbide nano particle and electrolyte.In document Nanoscale, 2014,
In 6,6151, Gao etc. is prepared for MoC/m-C combination electrode materials, compared to pure molybdenum carbide, the chemical property of the composite material
It is obviously improved.In 100mAg-1Under current density, for cycle after 50 weeks, the discharge capacity of MoC@C cathode can keep 670mAhg-1。
Although the molybdenum carbide nano particle that gas phase thermal reduction can be effectively evenly distributed, closed in order to which molybdenum is aoxidized
Object is fully heat-treated, and preparation process would generally use hazardous explosion prone gas, and there are certain security risks.For example, document
NanoLett.2015, in 15,5268, CH that Li is used4And H2Gaseous mixture prepares nanoscale MoC particles.Meanwhile ensure molybdenum oxidation
Close the key factor that object precursor is also synthesis nano molybdenum carbide particles in the fine dispersion of carbon base body.For this reason, it may be necessary to it uses
It can be with the good affine multi-pore channel structural material of molybdenum oxygen compound as reaction template.Not only long preparation period, but also synthesized
The control of journey is cumbersome, practical popularization and application of the limitation this method in industrial production.
For the problems in the relevant technologies, currently no effective solution has been proposed.
Invention content
For the above-mentioned technical problem in the relevant technologies, the present invention proposes that a kind of multilevel hierarchy molybdenum carbide/nitrogen-doped carbon is multiple
The preparation method of microballoon electrode material is closed, problems of the prior art can be solved.
To realize the above-mentioned technical purpose, the technical proposal of the invention is realized in this way：
A kind of preparation method of multilevel hierarchy molybdenum carbide/nitrogen-doped carbon complex microsphere electrode material, includes the following steps：
S1 lower stirring and dissolvings in the water of 30-60 DEG C of temperature by copper acetate, Pidolidone and phosphomolybdic acid；
S2 will descend stirring and dissolving in the water of 30-60 DEG C of temperature of melamine；
S3 mixes the solution in above-mentioned above-mentioned steps S1 and S2, is stirred to react 12-72h at being 50-90 DEG C in temperature, then takes out
It filters and washs filter cake with ethyl alcohol, in 50 DEG C of vacuum drying for 24 hours, obtain presoma；
Above-mentioned precursor is heated to 500-800 DEG C by S4 in an inert atmosphere, is slowly cooled to room temperature after isothermal holding 1-5 h,
Products therefrom is in FeCl360 DEG C of solution stirring 6h are filtered and with the filtered filter cake of pure water, by filter cake at a temperature of 80 DEG C
It is dried in vacuo 24 h.
Further, in step S1, the mass ratio of the copper acetate and Pidolidone is 2:1-5:1, copper acetate and phosphorus molybdenum
Sour mass ratio is 1:1-1:3, the mass ratio of phosphomolybdic acid and water is 1:100-1:200.
Further, in step S2, the mass ratio of the melamine and phosphomolybdic acid is 3:1-5:1, the melamine
Mass ratio with water is 1:40-1:100.
Further, in step S3, the rotating speed 1000-2000rpm of the stirring.
Further, in step S4, the inert gas is the mixing of the one or both of nitrogen and argon gas.
Further, in step S4, during the precursor heats in an inert atmosphere, heating rate 1-10
DEG C/min, the FeCl3Solution concentration is 0.5-2 mol/L.
Beneficial effects of the present invention：By the space confinement effect in carbon skeleton duct, the pyrolysis of melamine ligand discharges
Nitrogen-containing molecules slowly efficiently can carry out N doping to the table of molybdenum carbide particles/interface, enhance the storage lithium activity of molybdenum carbide；
Generated in-situ molybdenum carbide nano particle can not only combine closely with carbon substrate, and limited space effect also effectively inhibits carbonization
The high temperature agglomeration of molybdenum particle, so as to obtain the more uniform nano particle of dispersion, which shows higher
Specific capacity, good cycle performance and high rate performance, present invention process is simple, and cost of material is low, is easy to industrial scale production.
Description of the drawings
It in order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to institute in embodiment
Attached drawing to be used is needed to be briefly described, it should be apparent that, the accompanying drawings in the following description is only some implementations of the present invention
Example, for those of ordinary skill in the art, without creative efforts, can also obtain according to these attached drawings
Obtain other attached drawings.
Fig. 1 is the SEM figures for the composite material that embodiment one obtains；
Fig. 2 is the TEM figures for the composite material that embodiment two obtains；
Fig. 3 is the XPS figures of composite material N1s and Mo3d that embodiment three obtains；
Fig. 4 is the cycle performance figure for the composite material that example IV obtains.
Specific embodiment
Below in conjunction with the attached drawing in the embodiment of the present invention, the technical solution in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art's all other embodiments obtained belong to what the present invention protected
Range.
The system of a kind of multilevel hierarchy molybdenum carbide/nitrogen-doped carbon complex microsphere electrode material according to embodiments of the present invention
Preparation Method includes the following steps：
S1 lower stirring and dissolvings in the water of 30-60 DEG C of temperature by copper acetate, Pidolidone and phosphomolybdic acid；
S2 will descend stirring and dissolving in the water of 30-60 DEG C of temperature of melamine；
S3 mixes the solution in above-mentioned above-mentioned steps S1 and S2, is stirred to react 12-72h at being 50-90 DEG C in temperature, then takes out
It filters and washs filter cake with ethyl alcohol, in 50 DEG C of vacuum drying for 24 hours, obtain presoma；
Above-mentioned precursor is heated to 500-800 DEG C by S4 in an inert atmosphere, is slowly cooled to room temperature after isothermal holding 1-5 h,
Products therefrom is in FeCl360 DEG C of solution stirring 6h are filtered and with the filtered filter cake of pure water, by filter cake at a temperature of 80 DEG C
It is dried in vacuo 24 h.
In one particular embodiment of the present invention, in step S1, the mass ratio of the copper acetate and Pidolidone is 2:
1-5:1, copper acetate is 1 with phosphomolybdic acid mass ratio:1-1:3, the mass ratio of phosphomolybdic acid and water is 1:100-1:200.
In one particular embodiment of the present invention, in step S2, the mass ratio of the melamine and phosphomolybdic acid is 3:
1-5:1, the mass ratio of the melamine and water is 1:40-1:100.
In one particular embodiment of the present invention, in step S3, the rotating speed 1000-2000rpm of the stirring.
In one particular embodiment of the present invention, in step S4, the inert gas for nitrogen and argon gas one kind or
The two mixes.
In one particular embodiment of the present invention, in step S4, process that the precursor heats in an inert atmosphere
In, heating rate is 1-10 DEG C/min, the FeCl3Solution concentration is 0.5-2 mol/L.
In order to facilitate the above-mentioned technical proposal for understanding the present invention, below by way of specific embodiment to the above-mentioned technology of the present invention
Scheme is described in detail.
Embodiment one
0.35g copper acetates (analysis is pure), 0.12gL- glutamic acid (analysis is pure) and 0.55g phosphomolybdic acids (analysis is pure) is taken to be dissolved in 60mL
It in pure water, stirs and is completely dissolved at 60 DEG C, reaction solution A is made, 1.65g melamines (analysis is pure) is separately taken to be dissolved in 80mL pure water
In, it stirs and is completely dissolved at 60 DEG C, reaction solution B is made, treats that component is completely dissolved, in 1000rpm rotating speeds, 60 DEG C of stirred in water bath
48h is reacted, generation weak coffee color precipitation filters and washs filter cake with alcohol solvent, before 50 DEG C of vacuum drying obtain reaction afterwards for 24 hours
Body；Obtained precursor is placed in tubular heater, is heated to 600 DEG C in nitrogen atmosphere with the heating rate of 3 DEG C/min, heat preservation
It is slowly cooled to room temperature after processing 2h.Products therefrom is simultaneously filtered in 60 DEG C of stirring 6h of 2mol/LFeCl3 solution, suction filtration with pure water
Cake by filter cake in 80 DEG C of vacuum drying for 24 hours, obtains multilevel hierarchy molybdenum carbide/nitrogen-doped carbon complex microsphere electrode material.
SEM as shown in Figure 1 observes that multilevel hierarchy molybdenum carbide/nitrogen-doped carbon composite material of synthesis has the shape of micron ball
Looks.
Embodiment two
0.5g copper acetates (analysis is pure), 0.1gL- glutamic acid (analysis is pure) and 0.6g phosphomolybdic acids (analysis is pure) is taken to be dissolved in 78mL pure water
In, it stirs and is completely dissolved at 50 DEG C, reaction solution A is made, 1.8g melamines (analysis is pure) is separately taken to be dissolved in 100mL pure water,
Stirring is completely dissolved at 50 DEG C, and reaction solution B is made, treats that component is completely dissolved, in 1500rpm rotating speeds, 70 DEG C of stirred in water bath are anti-
Answer 48h, generation weak coffee color precipitation.It filters and washs filter cake with alcohol solvent, 50 DEG C of vacuum drying obtain reacting preceding body for 24 hours afterwards
Body；Obtained precursor is placed in tubular heater, 550 DEG C, at heat preservation are heated to the heating rate of 3 DEG C/min in argon atmospher
It is slowly cooled to room temperature after reason 3h.Products therefrom is simultaneously filtered in 60 DEG C of stirring 6h of 1mol/LFeCl3 solution, suction filtration with pure water
Cake by filter cake in 80 DEG C of vacuum drying for 24 hours, obtains multilevel hierarchy molybdenum carbide/nitrogen-doped carbon complex microsphere electrode material.
As shown in Fig. 2, in tem observation to the composite material of synthesis molybdenum carbide nano particle 3 ~ 5nm of grain size.
Embodiment three
0.3g copper acetates (analysis is pure), 0.1gL- glutamic acid (analysis is pure) and 0.39g phosphomolybdic acids (analysis is pure) is taken to be dissolved in 66mL pure
It in water, stirs and is completely dissolved at 55 DEG C, reaction solution A is made, 1.2g melamines (analysis is pure) is separately taken to be dissolved in 80mL pure water,
Stirring is completely dissolved at 55 DEG C, and reaction solution B is made, treats that component is completely dissolved, in 2000rpm rotating speeds, 80 DEG C of stirred in water bath are anti-
Answer 48h, generation weak coffee color precipitation.It filters and washs filter cake with alcohol solvent, 50 DEG C of vacuum drying obtain reacting preceding body for 24 hours afterwards
Body；Obtained precursor is placed in tubular heater, 750 DEG C, at heat preservation are heated to the heating rate of 5 DEG C/min in nitrogen atmosphere
It is slowly cooled to room temperature after reason 2h, products therefrom is in 2mol/LFeCl360 DEG C of stirring 6h of solution, filter and are filtered with pure water
Cake by filter cake in 80 DEG C of vacuum drying for 24 hours, obtains multilevel hierarchy molybdenum carbide/nitrogen-doped carbon complex microsphere electrode material.
As shown in figure 3, the XPS figures of N1s and Mo3d prove that nitrogen atom doping enters in carbon base body and molybdenum carbide.
Example IV
0.25g copper acetates (analysis is pure), 0.07gL- glutamic acid (analysis is pure) and 0.33g phosphomolybdic acids (analysis is pure) is taken to be dissolved in 82mL
It in pure water, stirs and is completely dissolved at 40 DEG C, reaction solution A is made, 1.32g melamines (analysis is pure) is separately taken to be dissolved in 92mL pure water
In, it stirs and is completely dissolved at 40 DEG C, reaction solution B is made.Treat that component is completely dissolved, in 1100rpm rotating speeds, 80 DEG C of stirred in water bath
48h is reacted, generation weak coffee color precipitation filters and washs filter cake with alcohol solvent, before 50 DEG C of vacuum drying obtain reaction afterwards for 24 hours
Body；Obtained precursor is placed in tubular heater, is added in mixed atmosphere (10%Ar+90N2) with the heating rate of 2 DEG C/min
Heat is slowly cooled to room temperature after isothermal holding 5h to 700 DEG C.Products therefrom is in 60 DEG C of stirring 6h of 1.5mol/LFeCl3 solution, pumping
It filters and uses pure water filter cake, by filter cake in 80 DEG C of vacuum drying for 24 hours.Obtain multilevel hierarchy molybdenum carbide/nitrogen-doped carbon complex microsphere
Electrode material.
Fig. 4 test results show that level structure molybdenum carbide/nitrogen-doped carbon complex microsphere has as lithium ion battery negative material
There is stable cycle performance.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.
Claims (6)
1. a kind of preparation method of multilevel hierarchy molybdenum carbide/nitrogen-doped carbon complex microsphere electrode material, which is characterized in that including with
Lower step：
S1 lower stirring and dissolvings in the water of 30-60 DEG C of temperature by copper acetate, Pidolidone and phosphomolybdic acid；
S2 will descend stirring and dissolving in the water of 30-60 DEG C of temperature of melamine；
S3 mixes the solution in above-mentioned above-mentioned steps S1 and S2, is stirred to react 12-72h at being 50-90 DEG C in temperature, then takes out
It filters and washs filter cake with ethyl alcohol, in 50 DEG C of vacuum drying for 24 hours, obtain presoma；
Above-mentioned precursor is heated to 500-800 DEG C by S4 in an inert atmosphere, is slowly cooled to room temperature after isothermal holding 1-5 h,
Products therefrom is in FeCl360 DEG C of solution stirring 6h are filtered and with the filtered filter cake of pure water, by filter cake at a temperature of 80 DEG C
It is dried in vacuo 24 h.
2. a kind of preparation side of multilevel hierarchy molybdenum carbide/nitrogen-doped carbon complex microsphere electrode material according to claim 1
Method, which is characterized in that in step S1, the mass ratio of the copper acetate and Pidolidone is 2:1-5:1, copper acetate and phosphomolybdic acid matter
Amount is than being 1:1-1:3, the mass ratio of phosphomolybdic acid and water is 1:100-1:200.
3. a kind of preparation side of multilevel hierarchy molybdenum carbide/nitrogen-doped carbon complex microsphere electrode material according to claim 2
Method, which is characterized in that in step S2, the mass ratio of the melamine and phosphomolybdic acid is 3:1-5:1, the melamine and water
Mass ratio be 1:40-1:100.
4. a kind of preparation side of multilevel hierarchy molybdenum carbide/nitrogen-doped carbon complex microsphere electrode material according to claim 3
Method, which is characterized in that in step S3, the rotating speed 1000-2000rpm of the stirring.
5. a kind of preparation side of multilevel hierarchy molybdenum carbide/nitrogen-doped carbon complex microsphere electrode material according to claim 4
Method, which is characterized in that in step S4, the inert gas is the mixing of the one or both of nitrogen and argon gas.
6. a kind of preparation side of multilevel hierarchy molybdenum carbide/nitrogen-doped carbon complex microsphere electrode material according to claim 5
Method, which is characterized in that in step S4, during the precursor heats in an inert atmosphere, heating rate for 1-10 DEG C/
Min, the FeCl3Solution concentration is 0.5-2 mol/L.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109590004A (en) * | 2018-12-13 | 2019-04-09 | 黑龙江大学 | A method of preparing molybdenum nitride-copper/graphene ternary complex |
| CN109794279A (en) * | 2019-02-22 | 2019-05-24 | 中国林业科学研究院林产化学工业研究所 | A kind of MoC/CN catalyst and preparation method thereof and the application in the reaction of oleic acid hydrogenation deoxidation |
| CN110265225A (en) * | 2019-05-23 | 2019-09-20 | 天津大学 | The method for preparing N doping three-dimensional porous carbosphere load molybdenum carbide/molybdenum nitride and iron nano-particle composite material |
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2017
- 2017-12-05 CN CN201711265228.3A patent/CN108183203A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109590004A (en) * | 2018-12-13 | 2019-04-09 | 黑龙江大学 | A method of preparing molybdenum nitride-copper/graphene ternary complex |
| CN109590004B (en) * | 2018-12-13 | 2021-09-24 | 黑龙江大学 | Method for preparing molybdenum nitride-copper/graphene ternary complex |
| CN109794279A (en) * | 2019-02-22 | 2019-05-24 | 中国林业科学研究院林产化学工业研究所 | A kind of MoC/CN catalyst and preparation method thereof and the application in the reaction of oleic acid hydrogenation deoxidation |
| CN109794279B (en) * | 2019-02-22 | 2022-04-05 | 中国林业科学研究院林产化学工业研究所 | MoC/CN catalyst, preparation method thereof and application thereof in oleic acid hydrodeoxygenation reaction |
| CN110265225A (en) * | 2019-05-23 | 2019-09-20 | 天津大学 | The method for preparing N doping three-dimensional porous carbosphere load molybdenum carbide/molybdenum nitride and iron nano-particle composite material |
| CN110265225B (en) * | 2019-05-23 | 2021-03-16 | 天津大学 | Method for preparing nitrogen-doped three-dimensional porous carbon microsphere loaded molybdenum carbide/molybdenum nitride and iron nanoparticle composite material |
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Application publication date: 20180619 |