CN109786666A - A kind of nitrogen-doped carbon coated Si nano particle composite material, preparation method and application - Google Patents
A kind of nitrogen-doped carbon coated Si nano particle composite material, preparation method and application Download PDFInfo
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- CN109786666A CN109786666A CN201910219250.7A CN201910219250A CN109786666A CN 109786666 A CN109786666 A CN 109786666A CN 201910219250 A CN201910219250 A CN 201910219250A CN 109786666 A CN109786666 A CN 109786666A
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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
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of nitrogen-doped carbon coated Si nano particle composite materials and preparation method thereof, the following steps are included: S1, by partial size being that 30~50nm nano silicon particles are placed in the Tris-HCl buffer solution that pH is 7.5, cleaning, it is dry, obtain processed nano silicon particles；S2, dopamine hydrochloride is added in the Tris-HCl buffer solution that pH is 8.5, dissolution obtains dopamine solution；S3, processed nano silicon particles obtained in S1 are added in dopamine solution obtained in S2, are uniformly dispersed, then at room temperature, be stirred to react 1~8 day, then separate, is dry, obtaining reactant；S4, under an inert atmosphere, the reactant that S3 is obtained is in 700~900 DEG C of 1~2h of calcining to get arriving composite material.The invention also discloses application of the above-mentioned composite material on cathode of lithium battery, the composite material that the present invention synthesizes has excellent cyclical stability.
Description
Technical field
The invention belongs to nano silicon particles modified composite material technical fields, and in particular to a kind of nitrogen-doped carbon coated Si is received
Rice grain composite material, preparation method and application.
Background technique
Negative electrode material is the extremely important component part of lithium ion battery, and the energy for directly influencing lithium ion battery is close
Degree and chemical property.The reversible capacity, cycle performance, high rate performance of lithium ion battery can be improved in excellent negative electrode material；
Otherwise it will cause the decaying of lithium ion performance, or even can not work.
Traditional graphite cathode material theoretical specific capacity is 372mAh/g, practical application material capacity up to 360mAh/g,
Almost without room for improvement；In contrast, silicon has high specific discharge capacity (4200mAh/g), it is graphite negative electrodes material
10 times or more.The theoretical capacity of SiO is also in 1400mAh or more.Use high performance silica-base material as negative electrode active material
One of most promising route of battery energy density is improved as current.But due to its in battery charge and discharge process due to following
Zernike annular polynomial generate volume deformation is larger and guiding discharge specific capacity rapid decay, the problem of cyclical stability difference.Although at present
There are also methods to provide the chemical property of silica-base material, but its operating method synthesis steps is complicated, and condition is harsh, at
This is higher.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of nitrogen-doped carbon coated Si nano-particles reinforcements
Material, preparation method and application.
The first purpose of the invention is to provide a kind of preparation method of nitrogen-doped carbon coated Si nano particle composite material,
The following steps are included:
S1, the nano silicon particles for being 30~50nm by partial size are placed in the Tris-HCl buffer solution that pH value is 7.5, clearly
It washes, it is dry, obtain processed nano silicon particles；
S2, dopamine hydrochloride is added in the Tris-HCl buffer solution that pH value is 8.5, it is molten to obtain dopamine for dissolution
Liquid；
S3, processed nano silicon particles obtained in S1 are added in dopamine solution obtained in S2, are uniformly dispersed,
Then at room temperature, it is stirred to react 1~8 day, then separates, is dry, obtaining reactant, wherein in nano silicon particles and S2
The mass ratio of dopamine hydrochloride is 100:8~80；
S4, under an inert atmosphere, the reactant that S3 is obtained is in 700~900 DEG C of 1~2h of calcining, cooled to room temperature,
Obtain nitrogen-doped carbon coated Si nano particle composite material.
Preferably, in step S2, the concentration of dopamine solution is 2mg/ml.
Preferably, in step S3, the revolving speed of stirring is 500r/min.
Preferably, in step S4, inert atmosphere is argon atmosphere.
Preferably, in step S4, the heating rate of calcination process is 5 DEG C/min.
A second object of the present invention is to provide a kind of nitrogen-doped carbon coated Si nanometers that above-mentioned preparation method is prepared
Particulate composite.
Third object of the present invention is to provide a kind of application of above-mentioned composite material on negative electrode of lithium ion battery.
Compared with prior art, the beneficial effects of the present invention are:
(1) present invention coats nano silicon particles by nitrogen-doped carbon and is modified to silica-base material, and operating method is simple, easily
In realization, low-carbon environment-friendly, cost is relatively low, is suitable for industrialized production and application；
(2) present invention is by regulating and controlling to being stirred to react the time, and then regulates and controls to the thickness of clad, thus right
The electrochemistry of the composite material of synthesis can be carried out regulation；
(3) composite material that the present invention synthesizes has good electric conductivity, can promote the electric conductivity of silica-base material, favorably
It is conducted in electronics, Heteroatom doping forms different Cloud Distributions and is also conducive to electronics conduction in clad, to lithium-ion electric
Constructing for pond negative electrode material electronic conduction path is of great significance；
(4) composite material that the present invention synthesizes recycles 50 circles under 500mA/g high current density, and specific capacity highest is still
1480mAh/g can be maintained, there is excellent electrochemistry cycle performance.
Detailed description of the invention
Fig. 1 is a kind of nitrogen-doped carbon coated Si nano particle composite material and comparative example 1 that 1-3 of the embodiment of the present invention is provided
Cycle performance curve graph of the silica-base material of offer under 500mA/g high current density；
Fig. 2 is a kind of nitrogen-doped carbon coated Si nano particle composite material and comparative example 2 that 4-6 of the embodiment of the present invention is provided
Cycle performance curve graph of the silica-base material of offer under 500mA/g high current density.
Specific embodiment
The specific embodiment of invention is described in detail with reference to the accompanying drawing, it is to be understood that protection model of the invention
It encloses and is not limited by the specific implementation.The test method of actual conditions is not specified in the following example, usually according to routine
Condition, or according to condition proposed by each manufacturer.
Embodiment 1
A kind of preparation method of nitrogen-doped carbon coated Si nano particle composite material, comprising the following steps:
S1, the nano silicon particles of 30nm are placed in the Tris-HCl buffer solution that pH value is 7.5, are sufficiently cleaned
(impurity of removal particle surface), it is dry, obtain processed nano silicon particles；
S2,0.1g dopamine hydrochloride is added in the Tris-HCl buffer solution that the pH value of 50ml is 8.5, dissolution obtains
To dopamine solution；
Processed nano silicon particles obtained in S3, the S1 by 0.1g are added in the S2 that 40ml concentration is 2mg/ml and obtain
Dopamine solution in, ultrasonic disperse is uniform, is transferred in the round-bottomed flask of 100ml, then at room temperature, in magnetic stirring apparatus
Upper setting revolving speed 500r/min, is stirred to react 1 day, is then centrifuged for separating, and in a vacuum drying oven in 60 DEG C of dry 12h, obtains
Reactant；
S4, under an argon atmosphere, for the reactant that S3 is obtained in 700 DEG C of calcining 2h, control heating rate is 5 DEG C/min,
Cooled to room temperature to get arrive nitrogen-doped carbon coated Si nano particle composite material.
Embodiment 2
The preparation method of nitrogen-doped carbon coated Si nano particle composite material provided in an embodiment of the present invention and embodiment 1
Preparation method is identical, and difference is only that, in step S3, being stirred to react the time is 4 days.
Embodiment 3
The preparation method of nitrogen-doped carbon coated Si nano particle composite material provided in an embodiment of the present invention and embodiment 1
Preparation method is identical, and difference is only that, in step S3, being stirred to react the time is 8 days.
Embodiment 4
The preparation method of nitrogen-doped carbon coated Si nano particle composite material provided in an embodiment of the present invention and embodiment 1
Preparation method is identical, and difference is only that, in step S1, the partial size of nano silicon particles is 50nm.
Embodiment 5
The preparation method of nitrogen-doped carbon coated Si nano particle composite material provided in an embodiment of the present invention and embodiment 2
Preparation method is identical, and difference is only that, in step S1, the partial size of nano silicon particles is 50nm.
Embodiment 6
The preparation method of nitrogen-doped carbon coated Si nano particle composite material provided in an embodiment of the present invention and embodiment 3
Preparation method is identical, and difference is only that, in step S1, the partial size of nano silicon particles is 50nm.
Embodiment 7
The preparation method of nitrogen-doped carbon coated Si nano particle composite material provided in an embodiment of the present invention and embodiment 1
Preparation method is identical, and difference is only that, in step S3, the additional amount of the dopamine solution of 2mg/ml is 8ml.
Embodiment 8
The preparation method of nitrogen-doped carbon coated Si nano particle composite material provided in an embodiment of the present invention and embodiment 1
Preparation method is identical, and difference is only that, in step S3, the additional amount of the dopamine solution of 2mg/ml is 4ml.
Embodiment 9
The preparation method of nitrogen-doped carbon coated Si nano particle composite material provided in an embodiment of the present invention and embodiment 1
Preparation method is identical, and difference is only that, in step S4, the temperature and time of calcining is respectively 900 DEG C and 1h.
Comparative example 1
The material that comparative example 1 provides is identical as the preparation method of composite material that embodiment 1 provides, and difference is only that, right
The material that ratio 1 provides does not pass through the processing of step S2-S4.
Comparative example 2
The material that comparative example 2 provides is identical as the preparation method of composite material that embodiment 4 provides, and difference is only that, right
The material that ratio 2 provides does not pass through the processing of step S2-S4.
Influence of the material prepared below to 1-6 of the embodiment of the present invention and comparative example 1 and 2 to chemical property is studied
1, electrochemical property test
The material that respectively prepares embodiment 1-6 and comparative example 1 and 2, carbon black, polyvinylidene fluoride according to 8:1:1 matter
Amount is matched and is ground after mixing with suitable N-Methyl pyrrolidone, electrode material is obtained, by electrode material coater
Coated on copper foil, in 80 DEG C of dry 3h, 12h is then dried in a vacuum drying oven, cell negative electrode material is obtained, in glove box
In using prepared negative electrode material as working electrode, lithium piece be to electrode, 1M LiPF6(ethylene carbonate, the carbon of 1:1 volume ratio
Dimethyl phthalate is mixed solvent) it is electrolyte, Celgard 2500 is diaphragm, is assembled into the button electricity of CR2025 model jointly
Pond.Then charge and discharge cycles test is carried out to the battery of assembling.
2, chemical property result
Fig. 1 is a kind of nitrogen-doped carbon coated Si nano particle composite material and comparative example 1 that 1-3 of the embodiment of the present invention is provided
Cycle performance curve graph of the silica-base material of offer under 500mA/g high current density.From figure 1 it appears that the present invention is real
Apply the cycle performance that a cycle performance for the composite material of 1-3 synthesis is superior to the silica-base material of the offer of comparative example 1, and embodiment
The composite material of 1 synthesis has more excellent cycle performance compared to embodiment 2 and 3, under 500mA/g high current density,
After 50 circle of circulation, reversible specific capacity is still up to 1480mAh/g, has good cyclic reversibility.
Fig. 2 is a kind of nitrogen-doped carbon coated Si nano particle composite material and comparative example 2 that 4-6 of the embodiment of the present invention is provided
Cycle performance curve graph of the silica-base material of offer under 500mA/g high current density.From figure 2 it can be seen that the present invention is real
Apply the cycle performance that a cycle performance for the composite material of 4-6 synthesis is superior to the silica-base material of the offer of comparative example 2, and embodiment
The composite material of 4 synthesis has more excellent cycle performance compared to embodiment 5 and 6, under 500mA/g high current density,
After 90 circle of circulation, reversible specific capacity is still up to 1080mAh/g, has good cyclic reversibility.
It is answered in conclusion the nitrogen-doped carbon coated Si nano particle composite material of synthesis of the embodiment of the present invention improves silicon substrate
The cyclical stability of condensation material, and when silica-base material partial size be 30nm, be stirred to react the time be 1 day when, have optimal electricity
Chemical property.
It should be noted that involved in claims of the present invention when numberical range, it is thus understood that each numberical range
Any one numerical value can be selected between two endpoints and two endpoints, since the step method of use is identical as embodiment,
It repeats in order to prevent, the present invention describes preferred embodiment and its effect, and once a person skilled in the art knows bases
This creative concept, then additional changes and modifications may be made to these embodiments.So the following claims are intended to be interpreted as
Including preferred embodiment and fall into all change and modification of the scope of the invention.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
Mind and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to include these modifications and variations.
Claims (7)
1. a kind of preparation method of nitrogen-doped carbon coated Si nano particle composite material, which comprises the following steps:
S1, the nano silicon particles for being 30~50nm by partial size are placed in the Tris-HCl buffer solution that pH value is 7.5, are cleaned, and are done
It is dry, obtain processed nano silicon particles；
S2, dopamine hydrochloride is added in the Tris-HCl buffer solution that pH value is 8.5, dissolution obtains dopamine solution；
S3, processed nano silicon particles obtained in S1 are added in dopamine solution obtained in S2, are uniformly dispersed, then
Reaction is stirred at room temperature 1~8 day, then separates, is dry, obtaining reactant, wherein is more in nano silicon particles and S2 in S1
The mass ratio of bar amine hydrochlorate is 100:8~80；
S4, under an inert atmosphere, the reactant that S3 is obtained in 700~900 DEG C of 1~2h of calcining, cooled to room temperature to get
To nitrogen-doped carbon coated Si nano particle composite material.
2. the preparation method of nitrogen-doped carbon coated Si nano particle composite material according to claim 1, which is characterized in that
In step S2, the concentration of the dopamine solution is 2mg/ml.
3. the preparation method of nitrogen-doped carbon coated Si nano particle composite material according to claim 1, which is characterized in that
In step S3, the revolving speed of the stirring is 500r/min.
4. the preparation method of nitrogen-doped carbon coated Si nano particle composite material according to claim 1, which is characterized in that
In step S4, the inert atmosphere is argon atmosphere.
5. the preparation method of nitrogen-doped carbon coated Si nano particle composite material according to claim 1, which is characterized in that
In step S4, the heating rate of the calcination process is 5 DEG C/min.
6. the preparation method of nitrogen-doped carbon coated Si nano particle composite material according to claim 1-5 obtains
Nitrogen-doped carbon coated Si nano particle composite material.
7. application of the composite material according to claim 6 on negative electrode of lithium ion battery.
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| CN110474034A (en) * | 2019-08-22 | 2019-11-19 | 陕西科技大学 | A kind of nitrogen mixes porous nano-sheet Si-C composite material and its preparation method and application |
| CN111149241A (en) * | 2019-12-30 | 2020-05-12 | 上海杉杉科技有限公司 | Silicon-based lithium storage material and preparation method thereof |
| CN111244430A (en) * | 2020-03-11 | 2020-06-05 | 武汉理工大学 | Silicon-carbon composite negative electrode material with double-wall core-shell structure and preparation and application thereof |
| CN112110448A (en) * | 2020-09-21 | 2020-12-22 | 中山大学 | Nitrogen-doped carbon and nano-silicon composite anode material and preparation method thereof |
| CN112467113A (en) * | 2020-12-01 | 2021-03-09 | 南昌大学 | Preparation method of nitrogen-doped carbon-coated silicon dioxide nanotube composite material |
| CN112635745A (en) * | 2019-10-09 | 2021-04-09 | 中国石油化工股份有限公司 | Composite material, preparation method thereof, lithium battery cathode and lithium battery |
| CN112670458A (en) * | 2019-10-16 | 2021-04-16 | 中国科学院福建物质结构研究所 | Preparation method and application of silicon-carbon material |
| CN113921794A (en) * | 2021-10-11 | 2022-01-11 | 福建蓝海黑石新材料科技有限公司 | Silicon-carbon composite material and preparation method and application thereof |
| CN114023953A (en) * | 2021-11-03 | 2022-02-08 | 惠州亿纬锂能股份有限公司 | Modified lithium iron manganese phosphate cathode material and preparation method and application thereof |
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|---|---|---|---|---|
| CN110474034A (en) * | 2019-08-22 | 2019-11-19 | 陕西科技大学 | A kind of nitrogen mixes porous nano-sheet Si-C composite material and its preparation method and application |
| CN112635745A (en) * | 2019-10-09 | 2021-04-09 | 中国石油化工股份有限公司 | Composite material, preparation method thereof, lithium battery cathode and lithium battery |
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| CN111244430A (en) * | 2020-03-11 | 2020-06-05 | 武汉理工大学 | Silicon-carbon composite negative electrode material with double-wall core-shell structure and preparation and application thereof |
| CN112110448A (en) * | 2020-09-21 | 2020-12-22 | 中山大学 | Nitrogen-doped carbon and nano-silicon composite anode material and preparation method thereof |
| CN112467113A (en) * | 2020-12-01 | 2021-03-09 | 南昌大学 | Preparation method of nitrogen-doped carbon-coated silicon dioxide nanotube composite material |
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| CN114023953A (en) * | 2021-11-03 | 2022-02-08 | 惠州亿纬锂能股份有限公司 | Modified lithium iron manganese phosphate cathode material and preparation method and application thereof |
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Application publication date: 20190521 |