CN110165164A - A kind of silicon-stratiform titanium carbide negative electrode material and preparation method thereof - Google Patents
A kind of silicon-stratiform titanium carbide negative electrode material and preparation method thereof Download PDFInfo
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- CN110165164A CN110165164A CN201910379289.5A CN201910379289A CN110165164A CN 110165164 A CN110165164 A CN 110165164A CN 201910379289 A CN201910379289 A CN 201910379289A CN 110165164 A CN110165164 A CN 110165164A
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- silicon
- titanium carbide
- negative electrode
- electrode material
- stratiform titanium
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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
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/366—Composites as layered products
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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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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- 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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- 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 invention discloses a kind of silicon-stratiform titanium carbide negative electrode materials and preparation method thereof, and the negative electrode material includes silicon particle and stratiform titanium carbide, and the silicon particle is evenly distributed between the sheet surfaces and lamella of stratiform titanium carbide.The preparation method comprises the following steps: by Ti3AlC2Or Ti3SiC2Etching in hydrogen fluoride solution is added and obtains stratiform titanium carbide；Stratiform titanium carbide and silicon particle are added in solvent and carry out ultrasonic disperse, obtains the silicon-stratiform titanium carbide negative electrode material after dry.Silicon proposed by the present invention-stratiform titanium carbide negative electrode material preparation method processing step is simple, and strong operability, obtained negative electrode material bulk effect is small, electric conductivity and good cycling stability.
Description
Technical field
The present invention relates to technical field of lithium ion more particularly to a kind of silicon-stratiform titanium carbide negative electrode materials and its system
Preparation Method.
Background technique
Energy density >=the 300KWh/g for currently requiring that single battery, the application for high energy density lithium ion, tradition
Graphite cathode material be no longer satisfied the requirement of energy density.Silicon based anode material theoretical capacity with higher, therefore
Silico-carbo negative electrode material starts to be applied to lithium ion battery negative material.But since silicon materials in charge and discharge process imitate by volume
Should be significant, when the content of silicon is more in silico-carbo composite material (> 20%), battery is in charge and discharge process caused by volume change
Stress makes negative electrode material dusting, is detached from collector, capacity diving.
Summary of the invention
Technical problems based on background technology, the invention proposes a kind of silicon-stratiform titanium carbide negative electrode material and its
Preparation method, the preparation method processing step is simple, strong operability, and obtained negative electrode material bulk effect is small, electric conductivity
Energy and good cycling stability.
A kind of silicon proposed by the present invention-stratiform titanium carbide negative electrode material, including silicon particle and stratiform titanium carbide, the silicon
Grain is evenly distributed between the sheet surfaces and lamella of stratiform titanium carbide.
Preferably, in silicon-stratiform titanium carbide negative electrode material, the mass fraction of the silicon particle is 5-40%.
Preferably, the silicon particle is silicon nanoparticle；The partial size of the silicon nanoparticle is 10-120 nanometers.
A kind of silicon-stratiform titanium carbide negative electrode material preparation method that the present invention also proposes, comprising the following steps:
S1, by Ti3AlC2Or Ti3SiC2Etching in hydrogen fluoride solution is added and obtains stratiform titanium carbide；
S2, ultrasonic disperse will be carried out in stratiform titanium carbide and silicon particle addition solvent, obtains the silicon-stratiform after dry
Titanium carbide negative electrode material.
Preferably, in S1, in the hydrogen fluoride solution, the mass fraction of hydrogen fluoride is 20-55%.
Preferably, in S1, the time of etching is 24-72 hours.
Preferably, in S2, the solvent is the mixing of one or more of water, ethyl alcohol, N-Methyl pyrrolidone
Object.
Preferably, in S2, the time of ultrasonic disperse is 5-60 minutes.
Preferably, in S2, dry temperature is 60-105 DEG C, and the dry time is 4-24 hours.
Silicon of the present invention-stratiform titanium carbide negative electrode material, including silicon particle and stratiform titanium carbide, the silicon particle are uniform
It is distributed between the sheet surfaces and lamella of stratiform titanium carbide, so that stratiform titanium carbide with good conductivity and silicon particle be carried out
It is compound, the bulk effect of silicon particle in the lithium intercalation/deintercalation process is buffered using the layer structure of stratiform titanium carbide, makes the silicon-
Stratiform titanium carbide negative electrode material bulk effect is small, and electric conductivity is good, good cycling stability；Preparation method work of the present invention
Skill step is simple, strong operability, and importing industrialization production for silica-base material has great importance.
Detailed description of the invention
Fig. 1 is silicon-stratiform titanium carbide negative electrode material structural schematic diagram in the embodiment of the present invention 1；
Fig. 2 is silicon-stratiform titanium carbide negative electrode material (silicon-stratiform titanium carbide) and commodity nanometer in the embodiment of the present invention 1
The circulation volume conservation rate curve of silicon particle (silicon nanoparticle).
Specific embodiment
In the following, technical solution of the present invention is described in detail by specific embodiment.
Embodiment 1
A kind of preparation method of silicon-stratiform titanium carbide negative electrode material proposed by the present invention, comprising the following steps:
S1, Ti is weighed3AlC2Powder 10g is added in the HF solution that 100g mass concentration is 40%, stirs 48 hours and carries out
Etching, obtains Ti3C2Suspension, the Ti that will be obtained3C2Suspension filtering, be dried to obtain stratiform titanium carbide；
It S2, is by weight that 20:80 is added in ethyl alcohol by silicon nanoparticle and stratiform titanium carbide, ultrasonic disperse 30min is obtained
To slurry, obtained slurry is filtered, then drying obtains the silicon-stratiform titanium carbide negative electrode material for 24 hours at 60 DEG C.
Fig. 1 is silicon-stratiform titanium carbide negative electrode material structural schematic diagram in the embodiment of the present invention 1；As shown in Figure 1, in silicon-
In stratiform titanium carbide negative electrode material, silicon nanoparticle is dispersed in surface and the interlayer of stratiform titanium carbide.
Take silicon obtained-stratiform titanium carbide negative electrode material, conductive black super P and binder sodium alginate by quality
It is mixed than 8:1:1, deionized water is added and is tuned into uniform slurry；Slurry is coated on copper foil of affluxion body, wherein coating thickness
It is 10 μm, is then placed in vacuum oven, it is 10 hours dry in vacuum environment, take out backlash electrode slice, electrode slice diameter
For 13mm.
The electric performance test of electrode slice sample carries out in 2032 type button cell systems, and electrolyte is that the LiPF6 of 1M is molten
Solution addition 1wt%VC (vinylene carbonate) EC/DEC (ethylene carbonate/diethyl carbonate, volume ratio 1:1) solution in,
It is metal lithium sheet to electrode.Above-mentioned button cell is connected in new prestige equipment, at room temperature, carries out constant current charge-discharge survey
Examination.First with the multiplying power discharging of 0.33C to stopping potential 0.01V (vs. Li/Li+), after standing 2min, then with times of 0.33C
Rate charges to stopping potential 1.0V (vs.Li/Li+), and obtained circulation volume conservation rate is as shown in Fig. 2, silicon-stratiform in i.e. Fig. 2
The curve that titanium carbide indicates, as shown in Figure 2, the capacity of silicon prepared by the present invention-stratiform titanium carbide negative electrode material 50 times circulations
Conservation rate is 85.5%, is significantly improved than commodity silicon nanoparticle (76.9%).
In the silicon-stratiform titanium carbide negative electrode material of the present embodiment, the gram volume of silicon materials is high, as main active material
Material；Stratiform titanium carbide capacity is lower, but its Layered-space can buffer the stress generated when the embedding lithium of silicon particle.Therefore, silicon-stratiform
Titanium carbide negative electrode material has both high capacity and cyclical stability.
Embodiment 2
A kind of preparation method of silicon-stratiform titanium carbide negative electrode material proposed by the present invention, comprising the following steps:
S1, Ti is weighed3AlC2Powder 10g is added in the HF solution that 150g mass concentration is 20%, stirs 72 hours, system
The suspension of standby stratiform titanium carbide out；Then by suspension filtering, the drying of stratiform titanium carbide, stratiform titanium carbide is obtained；
It S2, is by weight that 5:95 is added in ethyl alcohol by silicon nanoparticle and stratiform titanium carbide, ultrasonic disperse 5min takes out
Filter, then dry 4h obtains the silicon-stratiform titanium carbide negative electrode material at 105 DEG C.
Embodiment 3
A kind of silicon proposed by the present invention-stratiform titanium carbide negative electrode material, including silicon particle and stratiform titanium carbide, the silicon
Grain is evenly distributed between the sheet surfaces and lamella of stratiform titanium carbide.
A kind of preparation method of silicon-stratiform titanium carbide negative electrode material proposed by the present invention, comprising the following steps:
S1, Ti is weighed3SiC2Powder 10g is added in the HF solution that 100g mass concentration is 50%, stirs 24 hours, system
Standby stratiform Ti out3C2Suspension；Then by stratiform Ti3C2Suspension filtering, dry, obtain stratiform Ti3C2；
S2, the silicon nanoparticle and stratiform Ti that are 30-80nm by partial size3C2It is added in ethyl alcohol by weight 40:60, ultrasound
Disperse 60min, then filter, dry 13h obtains the silicon-stratiform titanium carbide negative electrode material at 80 DEG C.
Embodiment 4
A kind of silicon proposed by the present invention-stratiform titanium carbide negative electrode material, including silicon particle and stratiform titanium carbide, the silicon
Grain is evenly distributed between the sheet surfaces and lamella of stratiform titanium carbide.
A kind of silicon-stratiform titanium carbide negative electrode material preparation method that the present invention also proposes, comprising the following steps:
S1, by Ti3SiC2Etching in hydrogen fluoride solution is added and obtains stratiform titanium carbide；
S2, ultrasonic disperse will be carried out in stratiform titanium carbide and silicon particle addition solvent, obtains the silicon-stratiform after dry
Titanium carbide negative electrode material.
Embodiment 5
A kind of silicon proposed by the present invention-stratiform titanium carbide negative electrode material, including silicon nanoparticle and stratiform titanium carbide, it is described
Silicon nanoparticle is evenly distributed between the sheet surfaces and lamella of stratiform titanium carbide；Wherein, in silicon-stratiform titanium carbide cathode material
In material, the mass fraction of the silicon nanoparticle is 40%；The partial size of the silicon nanoparticle is 10-35 nanometers.
A kind of silicon-stratiform titanium carbide negative electrode material preparation method that the present invention also proposes, comprising the following steps:
S1, by Ti3AlC2It is added in the hydrogen fluoride solution that mass fraction is 55% and etches for 24 hours, obtain layer after filtering, drying
Shape titanium carbide；
S2, progress ultrasonic disperse 5min in ethyl alcohol is added in stratiform titanium carbide and silicon nanoparticle, at 105 DEG C after filtering
Lower dry 4h obtains the silicon-stratiform titanium carbide negative electrode material.
Embodiment 6
A kind of silicon proposed by the present invention-stratiform titanium carbide negative electrode material, including silicon particle and stratiform titanium carbide, the silicon
Grain is evenly distributed between the sheet surfaces and lamella of stratiform titanium carbide；Wherein, in silicon-stratiform titanium carbide negative electrode material, institute
The mass fraction for stating silicon particle is 5%；The silicon particle is silicon nanoparticle；The partial size of the silicon nanoparticle is received for 30-70
Rice.
A kind of silicon-stratiform titanium carbide negative electrode material preparation method that the present invention also proposes, comprising the following steps:
S1, by Ti3AlC2It is added in the hydrogen fluoride solution that mass fraction is 20% and etches 72h, obtain layer after filtering, drying
Shape titanium carbide；
S2, stratiform titanium carbide and silicon particle are added to the water to progress ultrasonic disperse 60min, it is dry at 60 DEG C after filtering
The silicon-stratiform titanium carbide negative electrode material is obtained for 24 hours.
Embodiment 7
A kind of silicon proposed by the present invention-stratiform titanium carbide negative electrode material, including silicon particle and stratiform titanium carbide, the silicon
Grain is evenly distributed between the sheet surfaces and lamella of stratiform titanium carbide；Wherein, in silicon-stratiform titanium carbide negative electrode material, institute
The mass fraction for stating silicon particle is 32%；The silicon particle is silicon nanoparticle；The partial size of the silicon nanoparticle is 10-120
Nanometer.
A kind of silicon-stratiform titanium carbide negative electrode material preparation method that the present invention also proposes, comprising the following steps:
S1, by Ti3AlC2It is added in the hydrogen fluoride solution that mass fraction is 40% and etches 55h, obtain layer after filtering, drying
Shape titanium carbide；
S2, it will carry out ultrasonic disperse 38 minutes in stratiform titanium carbide and silicon particle addition solvent, done at 80 DEG C after filtering
Obtain within dry 13 hours the silicon-stratiform titanium carbide negative electrode material；Wherein, the solvent is the mixture of water, ethyl alcohol.
Embodiment 8
A kind of silicon proposed by the present invention-stratiform titanium carbide negative electrode material, including silicon particle and stratiform titanium carbide, the silicon
Grain is evenly distributed between the sheet surfaces and lamella of stratiform titanium carbide；Wherein, in silicon-stratiform titanium carbide negative electrode material, institute
The mass fraction for stating silicon particle is 18%；The silicon particle is silicon nanoparticle；The partial size of the silicon nanoparticle is 70-115
Nanometer.
A kind of silicon-stratiform titanium carbide negative electrode material preparation method that the present invention also proposes, comprising the following steps:
S1, by Ti3SiC2Etching in hydrogen fluoride solution is added and obtains stratiform titanium carbide；Wherein, in the hydrogen fluoride solution,
The mass fraction of hydrogen fluoride is 28%；The time of etching is 33 hours；
S2, ultrasonic disperse will be carried out in stratiform titanium carbide and silicon particle addition solvent, obtains the silicon-stratiform after dry
Titanium carbide negative electrode material；Wherein, the solvent is the mixture of water, N-Methyl pyrrolidone；The time of ultrasonic disperse is 47 points
Clock；Dry temperature is 95 DEG C, and the dry time is 18 hours.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (9)
1. a kind of silicon-stratiform titanium carbide negative electrode material, which is characterized in that including silicon particle and stratiform titanium carbide, the silicon particle
It is evenly distributed between the sheet surfaces and lamella of stratiform titanium carbide.
2. silicon-stratiform titanium carbide negative electrode material according to claim 1, which is characterized in that in silicon-stratiform titanium carbide cathode material
In material, the mass fraction of the silicon particle is 5-40%.
3. silicon according to claim 1 or claim 2-stratiform titanium carbide negative electrode material, which is characterized in that the silicon particle is nano-silicon
Particle；The partial size of the silicon nanoparticle is 10-120 nanometers.
4. a kind of silicon as described in any one of claim 1-3-stratiform titanium carbide negative electrode material preparation method, feature exist
In, comprising the following steps:
S1, by Ti3AlC2Or Ti3SiC2Etching in hydrogen fluoride solution is added and obtains stratiform titanium carbide；
S2, ultrasonic disperse will be carried out in stratiform titanium carbide and silicon particle addition solvent, obtains the silicon-stratiform titanium carbide after dry
Negative electrode material.
5. silicon-stratiform titanium carbide negative electrode material preparation method according to claim 4, which is characterized in that described in S1
In hydrogen fluoride solution, the mass fraction of hydrogen fluoride is 20-55%.
6. silicon according to claim 4 or 5-stratiform titanium carbide negative electrode material preparation method, which is characterized in that in S1,
The time of etching is 24-72 hours.
7. the silicon according to any one of claim 4-6-stratiform titanium carbide negative electrode material preparation method, which is characterized in that
In S2, the solvent is the mixture of one or more of water, ethyl alcohol, N-Methyl pyrrolidone.
8. the silicon according to any one of claim 4-7-stratiform titanium carbide negative electrode material preparation method, which is characterized in that
In S2, the time of ultrasonic disperse is 5-60 minutes.
9. the silicon according to any one of claim 4-8-stratiform titanium carbide negative electrode material preparation method, which is characterized in that
In S2, dry temperature is 60-105 DEG C, and the dry time is 4-24 hours.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113943003A (en) * | 2021-11-09 | 2022-01-18 | 滁州学院 | With Ti3SiC2Preparation of two-dimensional Material Ti for precursor3C2Method (2) |
| CN114050234A (en) * | 2021-11-15 | 2022-02-15 | 珠海冠宇电池股份有限公司 | Negative plate and lithium ion battery comprising same |
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| CN107394180A (en) * | 2017-08-04 | 2017-11-24 | 南京工业大学 | Two-dimentional magnesium-yttrium-transition metal carbon (nitrogen) compound silicon nanoparticle composite and preparation and application |
| CN107492641A (en) * | 2017-07-31 | 2017-12-19 | 安阳工学院 | A kind of titanium carbide four vulcanizes three titanium composite materials and preparation method thereof |
| CN109346681A (en) * | 2018-08-17 | 2019-02-15 | 福建翔丰华新能源材料有限公司 | A kind of nuclear shell structure nano silicon-MXene composite negative pole material and preparation method thereof |
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2019
- 2019-05-08 CN CN201910379289.5A patent/CN110165164A/en active Pending
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| AU2007215394A1 (en) * | 2006-02-17 | 2007-08-23 | Gravitas Technologies Pty Ltd | Crystalline ternary ceramic precursors |
| CN107492641A (en) * | 2017-07-31 | 2017-12-19 | 安阳工学院 | A kind of titanium carbide four vulcanizes three titanium composite materials and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113943003A (en) * | 2021-11-09 | 2022-01-18 | 滁州学院 | With Ti3SiC2Preparation of two-dimensional Material Ti for precursor3C2Method (2) |
| CN114050234A (en) * | 2021-11-15 | 2022-02-15 | 珠海冠宇电池股份有限公司 | Negative plate and lithium ion battery comprising same |
| CN114050234B (en) * | 2021-11-15 | 2023-02-28 | 珠海冠宇电池股份有限公司 | Negative plate and lithium ion battery comprising same |
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Application publication date: 20190823 |