CN109360957A - A kind of preparation method of the carbon-based kalium ion battery negative electrode material of nitrogen oxygen auto-dope - Google Patents
A kind of preparation method of the carbon-based kalium ion battery negative electrode material of nitrogen oxygen auto-dope Download PDFInfo
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- CN109360957A CN109360957A CN201811168987.2A CN201811168987A CN109360957A CN 109360957 A CN109360957 A CN 109360957A CN 201811168987 A CN201811168987 A CN 201811168987A CN 109360957 A CN109360957 A CN 109360957A
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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
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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
- H01M4/58—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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- 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
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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
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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- 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 methods of the carbon-based kalium ion battery negative electrode material of nitrogen oxygen auto-dope, it has the feature that, the following steps are included: step 1, weigh oxide salt, oxide salt is dissolved in solvent, the ultrasonic treatment that 15-45 minutes are then carried out in 20 DEG C -30 DEG C of environment, obtains oxide salt solution；Step 2, oxide salt solution is uniformly laid in substrate, then substrate is placed on 40 DEG C -70 DEG C of warm table after heating 20-40 seconds and obtains one layer of uniform oxidant film in substrate；Step 3, substrate and oxidant film are placed in the air-tight bottle full of pyrroles's steam, make pyrrole monomer and oxidant film that polymerization reaction occur, reaction obtains polypyrrole film after continuing 0.5-24 hours in substrate；Step 4, polypyrrole film is placed in inertia or reducibility gas from removing in substrate, then obtains the carbon-based kalium ion battery negative electrode material of nitrogen oxygen auto-dope after 500 DEG C -1000 DEG C of environment high temperature is carbonized 0.5-24 hours.
Description
Technical field
The invention belongs to electric material technical fields, and in particular to a kind of carbon-based kalium ion battery cathode of nitrogen oxygen auto-dope
The preparation method of material.
Background technique
Information-based, automation modern society is constantly progressive, and people are also increasing for the demand of the energy, in this background
Under, electrochemical energy storage technology has obtained development at full speed.Lithium ion battery is big etc. excellent because having small in size, light weight, specific capacity
Gesture and be widely used, but content of the lithium resource in the earth's crust is only 0.0065%, so that lithium ion battery cost is not
It is disconnected to rise, there is property similar with lithium with the potassium (2.47%) and sodium (2.74%) element of main group but earth's crust rich content with lithium
Matter and it is abundant, widely distributed more than lithium resource, be easy to obtain, therefore to have obtained people more next for kalium ion battery and sodium-ion battery
More concerns.
Sodium-ion battery is because of its standard electrode EMF (- 2.71V) and big ionic radius limitation, so that energy density and function
Still there is a big difference compared with lithium ion battery for rate density.In addition, theoretical calculation and experiments have shown that sodium ion be difficult be embedded in graphite formed
Stable intercalation compound, and the standard electrode EMF (- 3.04V) of the closer lithium of the standard electrode EMF (- 2.93V) of potassium, and
The potassium of graphite is the most stable form that alkali metal insertion graphite linings are formed, its stability is even than graphite as lithium-ion electric
The stability in pond is more preferable, therefore commercialized graphite cathode material can be applied directly in kalium ion battery.But full of potassium
The theoretical volume of graphite is expanded to 61%, and capacity is only after kalium ion battery graphite cathode recycles 50 circles under the current density of 0.5C
It is maintained at 50% or so, big volume expansion may be the main reason for causing graphite cyclical stability poor.Additionally due to potassium compared with
Big ionic radius, so that kalium ion battery graphite cathode high rate performance is poor.
In recent years, researcher has carried out a large amount of scientific research to solve the above-mentioned problems, to improve kalium ion battery carbon
The capacity and high rate performance of negative electrode material, but these problems still fail to obtain effective solution.
Summary of the invention
The present invention be to solve the above-mentioned problems and carry out, and it is an object of the present invention to provide a kind of carbon-based potassium of nitrogen oxygen auto-dope from
The preparation method of sub- cell negative electrode material.
The present invention provides a kind of preparation methods of the carbon-based kalium ion battery negative electrode material of nitrogen oxygen auto-dope, have in this way
Feature, comprising the following steps: step 1, weigh oxide salt, oxide salt be dissolved in volatile solvent, then 20
The ultrasonic treatment carried out 15-45 minutes in DEG C -30 DEG C of environment is aoxidized so that oxide salt is substantially dissolved in solvent
Object salting liquid；
Step 2, oxide salt solution is uniformly laid in substrate, substrate is then placed in 40 DEG C -70 DEG C of heating
It heats 20-40 seconds, is waited after the solvent is volatilized on platform, one layer of uniform oxidant film is obtained in substrate；
Step 3, substrate and oxidant film are placed in the air-tight bottle full of pyrroles's steam, make pyrrole monomer and oxidant
Polymerization reaction occurs for film, and reaction obtains polypyrrole film after continuing 0.5-24 hours in substrate；
Step 4, polypyrrole film is placed in inertia or reducibility gas from removing in substrate, then at 500 DEG C -1000
DEG C environment high temperature be carbonized 0.5-24 hours after obtain a kind of carbon-based kalium ion battery negative electrode material of nitrogen oxygen auto-dope.
In a kind of preparation method of the carbon-based kalium ion battery negative electrode material of nitrogen oxygen auto-dope provided by the invention, may be used also
To have a feature in that wherein, in step 1, oxide salt is P- toluene fulfonate, benzene sulfonate, 4- ethyl group benzene sulfonic acid
Salt, 4-N- octyl benzene sulfonic acid salt, dodecyl benzene sulfonate, 1,3,3- tri-methyl p-toluenesulfonate salt, m- dimethylbenzene -4- sulfonate,
Etamon-P- toluenesulfonate or thiosulfate.
In a kind of preparation method of the carbon-based kalium ion battery negative electrode material of nitrogen oxygen auto-dope provided by the invention, may be used also
To have a feature in that wherein, in step 1, mass fraction of the oxide salt in oxide salt solution is 5%-95%.
In a kind of preparation method of the carbon-based kalium ion battery negative electrode material of nitrogen oxygen auto-dope provided by the invention, may be used also
To have a feature in that wherein, in step 1, volatile solvent is water, methanol, ethyl alcohol, ethylene glycol, acetonitrile, ether or just
Butanol.
In a kind of preparation method of the carbon-based kalium ion battery negative electrode material of nitrogen oxygen auto-dope provided by the invention, may be used also
To have a feature in that wherein, in step 2, substrate is glass, quartz, mica, ceramics, plastics or metal.
In a kind of preparation method of the carbon-based kalium ion battery negative electrode material of nitrogen oxygen auto-dope provided by the invention, may be used also
To have a feature in that wherein, in step 4, the method that polypyrrole film is removed from substrate for mechanical stripping or is placed in
Immersion removing is carried out in ionized water, methanol, ethyl alcohol, ethylene glycol, acetonitrile, ether or n-butanol.
The action and effect of invention
A kind of preparation method of the carbon-based kalium ion battery negative electrode material of nitrogen oxygen auto-dope involved according to the present invention is led to
It crosses using pyrrole monomer and oxidant as raw material, is had using gas-phase polymerization self assembly and heat-treating methods to be prepared
The carbon-based kalium ion battery negative electrode material of the nitrogen oxygen auto-dope of three-dimensional cross-linked reticular structure, the three-dimensional cross-linked reticular structure provide
The fast transferring channel of electronics and ion ensures excellent high rate performance, and potassium ion can be effectively relieved in embedding de- process
In volume expansion problem, the cyclical stability of kalium ion battery is promoted with this.Meanwhile N and O codope can not only influence carbon
The equilibrium state of electronics in structure, moreover it is possible to form stable C-N key and C-O key at high temperature, the C-N key and C-O key can not only
Increase carbon-coating spacing, and more defects and active site can be provided, to further promote the specific volume of kalium ion battery
Amount.And a kind of preparation method simple process of the carbon-based kalium ion battery negative electrode material of nitrogen oxygen auto-dope of the invention, preparation are used
When short and do not need that special installation, yield are high, controllability is good, and the equal asepsis environment-protecting of raw material, can be realized large-scale life
It produces.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of the carbon-based kalium ion battery negative electrode material of the nitrogen oxygen auto-dope of the embodiment of the present invention；
Fig. 2 is the transmission electron microscope photo of the carbon-based kalium ion battery negative electrode material of the nitrogen oxygen auto-dope of the embodiment of the present invention；
Fig. 3 is the carbon-based kalium ion battery negative electrode material of the nitrogen oxygen auto-dope of the embodiment of the present invention in 100mA g-1Electric current
Specific capacity and cycle efficieny figure under density；
Fig. 4 is the carbon-based kalium ion battery negative electrode material of the nitrogen oxygen auto-dope of the embodiment of the present invention in 1000mA g-1Electricity
Specific capacity and cycle efficieny figure under current density；
Fig. 5 is the carbon-based kalium ion battery negative electrode material of the nitrogen oxygen auto-dope of the embodiment of the present invention in 0.05A g-1~2A
g-1Current density under discharge capacity curve graph.
Specific embodiment
In order to which the technological means for realizing the present invention is easy to understand with effect, with reference to embodiments and attached drawing is to this
Invention is specifically addressed.
<embodiment>
The preparation method of the carbon-based kalium ion battery negative electrode material of nitrogen oxygen auto-dope in the present embodiment, including following step
It is rapid:
Step 1, P- toluene fulfonate is chosen as oxide salt, chooses n-butanol as solvent, by P- toluene fulfonate
It is dissolved in n-butanol, the ultrasonic treatment then carried out 30 minutes at room temperature obtains so that oxide salt is substantially dissolved in solvent
The P- tosylate solutions that the mass fraction of P- toluene fulfonate is 40% in solution.
Step 2, P- tosylate solutions are uniformly tiled on the glass sheet, then by sheet glass be placed in 50 DEG C plus
It is heated 20 seconds in thermal station, after waiting n-butanol volatilization, the oxidant film of one layer of uniform P- toluenesulfonic acid iron is obtained in substrate.
Step 3, sheet glass and oxidant film are placed in the air-tight bottle full of pyrroles's steam after standing 1 hour obtain it is black
The polypyrrole film of color.
Step 4, the polypyrrole film of the black is placed to be placed in ethyl alcohol within 1 hour at room temperature and carries out immersion removing, it will
700 DEG C are warming up to the heating rate of 5 DEG C/min under the protection of nitrogen after polypyrrole film removing, the high temperature cabonization 2 at 700 DEG C
The carbon-based kalium ion battery negative electrode material of nitrogen oxygen auto-dope is made after hour.
The carbon-based kalium ion battery negative electrode material of nitrogen oxygen auto-dope obtained is assembled into potassium ion half-cell, assembling process
It is as follows: by the binder (concentration of the carbon-based kalium ion battery negative electrode material of the nitrogen oxygen auto-dope of preparation and mass fraction 10wt%
For 0.04g ml-1Kynoar solution) and 10wt% conductive agent (SuperP) mixing, add appropriate NMP and stir evenly
It is coated on copper foil afterwards.Copper foil is cut into the electrode slice that diameter is 12mm after drying 1 hour, electrode slice is put into 80 DEG C true
Dry 12h, is then transferred to assembled battery in the glove box full of high-purity argon gas in empty baking oven.It is pair with bright metallic potassium piece
Electrode uses fibreglass diaphragm, 1molL-1Ethylene carbonate, the dimethyl carbonate (volume ratio 1:1) of Potassium Hexafluorophosphate are mixed
Conjunction solution is electrolyte, is assembled into CR2032 button cell, and the survey of constant current charge-discharge performance is carried out on LAND battery test system
Examination, charge and discharge blanking voltage are 0.01~3V.
The action and effect of embodiment
Fig. 1 is the scanning electron microscope (SEM) photograph of the carbon-based kalium ion battery negative electrode material of the nitrogen oxygen auto-dope of the embodiment of the present invention, Fig. 2
It is the transmission electron microscope photo of the carbon-based kalium ion battery negative electrode material of the nitrogen oxygen auto-dope of the embodiment of the present invention.
As depicted in figs. 1 and 2, the carbon-based kalium ion battery negative electrode material for the nitrogen oxygen auto-dope being prepared has three-dimensional hand over
Join reticular structure.
Fig. 3 is the carbon-based kalium ion battery negative electrode material of the nitrogen oxygen auto-dope of the embodiment of the present invention in 100mA g-1Electric current
Specific capacity and cycle efficieny figure under density, Fig. 4 are the carbon-based kalium ion battery cathode of the nitrogen oxygen auto-dope of the embodiment of the present invention
Material is in 1000mA g-1Current density under specific capacity and cycle efficieny figure.
As shown in Figure 3 and Figure 4, the carbon-based kalium ion battery negative electrode material for the nitrogen oxygen auto-dope being prepared is in 100mA g-1
Current density under circulation 500 circle after be able to maintain 241mAh g-1Height ratio capacity, in 1000mA g-1High current density under follow
Ring 1000 is also able to maintain 174mAh g after enclosing-1Specific capacity.
Fig. 5 is the carbon-based kalium ion battery negative electrode material of the nitrogen oxygen auto-dope of the embodiment of the present invention in 0.05A g-1~2A
g-1Current density under discharge capacity curve graph.
As shown in figure 5, the carbon-based kalium ion battery negative electrode material for the nitrogen oxygen auto-dope being prepared is in 0.05A g-1~2A
g-1Between different current densities under can guarantee good discharge capacity.
In conclusion the carbon-based kalium ion battery negative electrode material of the nitrogen oxygen auto-dope of the present embodiment is with three-dimensional cross-linked netted
Structure, which can increase the electric conductivity of ion and battery, and three-dimensional cross-linked reticular structure has centainly
Flexibility, carbon negative pole material can be alleviated in expansion issues during potassium ion deintercalation, to promote kalium ion battery
Cyclical stability.Meanwhile the carbon-based kalium ion battery negative electrode material of the nitrogen oxygen auto-dope has excellent high rate performance, Neng Goushi
It answers the charge and discharge cycles of different current densities to test, and there is good chemical property, potassium ion electricity can be effectively improved
The capacity in pond, the service life for extending kalium ion battery.And the carbon-based kalium ion battery cathode of the nitrogen oxygen auto-dope of the present embodiment
The simple process of the preparation method of material, preparation used time are short and do not need that special installation, yield are high, controllability is good, and former material
Expect equal asepsis environment-protecting, can be realized large-scale production.
Above embodiment is preferred case of the invention, the protection scope being not intended to limit the invention.
Claims (6)
1. a kind of preparation method of the carbon-based kalium ion battery negative electrode material of nitrogen oxygen auto-dope, which is characterized in that including following step
It is rapid:
Step 1, oxide salt is weighed, the oxide salt is dissolved in volatile solvent, then in 20 DEG C -30 DEG C of environment
The middle ultrasonic treatment carried out 15-45 minutes obtains oxide salt solution so that the oxide salt is substantially dissolved in solvent；
Step 2, the oxide salt solution is uniformly laid in substrate, the substrate is then placed in 40 DEG C -70 DEG C
It is heated 20-40 seconds on warm table, after waiting the solvent to volatilize, obtains one layer of uniform oxidant film on the substrate；
Step 3, the substrate and the oxidant film are placed in the air-tight bottle full of pyrroles's steam, make pyrrole monomer and institute
It states oxidant film and polymerization reaction occurs, reaction obtains polypyrrole film after continuing 0.5-24 hours on the substrate；
Step 4, the polypyrrole film is placed in inertia or reducibility gas from removing in the substrate, then 500 DEG C-
1000 DEG C of environment high temperature obtains the carbon-based kalium ion battery negative electrode material of nitrogen oxygen auto-dope after being carbonized 0.5-24 hours.
2. a kind of preparation method of the carbon-based kalium ion battery negative electrode material of nitrogen oxygen auto-dope according to claim 1,
It is characterized in that:
Wherein, in the step 1, oxide salt is P- toluene fulfonate, benzene sulfonate, 4- ethyl group benzene sulfonate, 4-N- pungent
Base benzene sulfonate, dodecyl benzene sulfonate, 1,3,3- tri-methyl p-toluenesulfonate salt, m- dimethylbenzene -4- sulfonate, etamon-P-
Toluenesulfonate or thiosulfate.
3. a kind of preparation method of the carbon-based kalium ion battery negative electrode material of nitrogen oxygen auto-dope according to claim 1,
It is characterized in that:
Wherein, in the step 1, mass fraction of the oxide salt in oxide salt solution is 5%-95%.
4. a kind of preparation method of the carbon-based kalium ion battery negative electrode material of nitrogen oxygen auto-dope according to claim 1,
It is characterized in that:
Wherein, in the step 1, volatile solvent is water, methanol, ethyl alcohol, ethylene glycol, acetonitrile, ether or n-butanol.
5. a kind of preparation method of the carbon-based kalium ion battery negative electrode material of nitrogen oxygen auto-dope according to claim 1,
It is characterized in that:
Wherein, in the step 2, substrate is glass, quartz, mica, ceramics, plastics or metal.
6. a kind of preparation method of the carbon-based kalium ion battery negative electrode material of nitrogen oxygen auto-dope according to claim 1,
It is characterized in that:
Wherein, in the step 4, the method that polypyrrole film is removed from substrate for mechanical stripping or is placed in deionized water, first
Immersion removing is carried out in alcohol, ethyl alcohol, ethylene glycol, acetonitrile, ether or n-butanol.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110571423A (en) * | 2019-09-17 | 2019-12-13 | 上海理工大学 | Preparation method of nitrogen-carbon-coated nano titanium niobate electrode material |
| CN113659143A (en) * | 2021-08-06 | 2021-11-16 | 东莞市创明电池技术有限公司 | Preparation method of negative electrode material of sodium ion battery, negative electrode material and sodium ion battery |
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| CN106025183A (en) * | 2016-05-19 | 2016-10-12 | 上海理工大学 | Preparation method of carbon-based flexible film electrode for lithium ion batteries |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110571423A (en) * | 2019-09-17 | 2019-12-13 | 上海理工大学 | Preparation method of nitrogen-carbon-coated nano titanium niobate electrode material |
| CN113659143A (en) * | 2021-08-06 | 2021-11-16 | 东莞市创明电池技术有限公司 | Preparation method of negative electrode material of sodium ion battery, negative electrode material and sodium ion battery |
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Application publication date: 20190219 |