CN108365184A - A kind of lithium ion battery porous SiOC negative materials of rich carbon and preparation method thereof - Google Patents
A kind of lithium ion battery porous SiOC negative materials of rich carbon and preparation method thereof Download PDFInfo
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- CN108365184A CN108365184A CN201810002156.1A CN201810002156A CN108365184A CN 108365184 A CN108365184 A CN 108365184A CN 201810002156 A CN201810002156 A CN 201810002156A CN 108365184 A CN108365184 A CN 108365184A
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- H01M4/00—Electrodes
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- H—ELECTRICITY
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- 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
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- H—ELECTRICITY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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Abstract
The present invention provides a kind of lithium ion battery porous SiOC cathode material preparation methods of rich carbon, include the following steps：By biomass waste after crushing, sieving ball milling, then take out drying；Organic siliconresin and biomass waste powder are mixed, and organic solution is added as solvent, so that biomass waste powder is sufficiently impregnated organic silicones using heating magnetic agitation, then drying obtains the mixture of organic siliconresin and biomass waste powder；Mixture is placed in tube furnace, under inert gas protection high temperature sintering, sintering temperature is 800~1100 DEG C, then furnace cooling after keeping the temperature；It is dry after being performed etching to obtained SiOC ceramic powders using strong base solution；Ceramic powder is placed in tube furnace, carries out activation heat treatment under inert gas protection, is then taken out and is boiled in deionized water, is washed to re-dry after neutrality.The problems such as present invention can solve the height of irreversible capacity for the first time with lithium ion battery SiOC negative materials, cyclical stability is poor.
Description
Technical field
The present invention relates to function ceramics preparing technical field and field of lithium, more particularly to a kind of for assembling lithium ion
Battery porous SiOC negative materials of rich carbon and preparation method thereof.
Background technology
With electronic technology, the rapid development of science and techniques of defence and a large amount of novel portable electronic products and electric tool
It develops, people propose increasingly higher demands to electrochmical power source especially high-performance secondary cell.Lithium rechargeable battery by
In energy density height, good cycle, the pollution-free advantages of nontoxic raw materials the features such as and by the extensive concern of researcher.Commercialization at present
Lithium ion battery mainly use graphite-like carbon material as negative material, but as lithium ion battery exists as power battery
The fast development and application of hybrid electric vehicle and portable electronic device, graphite negative electrodes materials theory specific capacity (372mAh/g)
Relatively low disadvantage is increasingly protruded, therefore the new type lithium ion electricity of a kind of height ratio capacity of exploitation, long circulation life and high performance-price ratio
Pond negative material has important practical significance.
From J.R.Dahn et al. SiOC ceramics are prepared by being pyrolyzed polysilane, polysiloxanes and silane-asphalt mixture
Powder, and SiOC ceramics are found with after good chemical property, which becomes cathode material of lithium ion battery field
The hot spot competitively studied.Although the reversible specific capacity of SiOC negative materials is be commercialized graphite-like carbon material nearly 3 times, the material
The irreversible capacity for the first time of material is higher and the shortcomings that there are voltage delay, be can be formed in telescopiny due to Li+ it is irreversible
Li2O and Li4SiO4, cause the irreversible capacity for the first time of the material higher；In subsequent cycle, which shows electricity
Pressure lag, i.e., de- lithium need higher voltage, a main inducing part to derive from the dynamics such as polarization caused by electric current than embedding lithium
Factor, a part come from lithium ion and wait Thermodynamics to the diffusion of SiOC active materials is hindered, finally affect SiOC
The cyclical stability of negative material.
Invention content
In response to the deficiencies in the existing technology, it is porous for assembling the rich carbon of lithium ion battery that the present invention provides one kind
SiOC negative materials and preparation method thereof solve the height of irreversible capacity for the first time, the cycle of lithium ion battery SiOC negative materials
The problems such as stability is poor, and a kind of preparation method of the porous SiOC negative materials of rich carbon of lithium ion battery is provided, and raw material comes
Source range is extensive, simple for process, and cost is relatively low.
The present invention achieves the above technical objects by the following technical means.
A kind of lithium ion battery porous SiOC cathode material preparation methods of rich carbon, include the following steps：
S01：By biomass waste after crushing, sieving ball milling, then take out drying；It will treated biomass waste
Grain size is taken to be less than 64 μm of biomass waste powder after screening；
S02：Organic siliconresin and biomass waste powder are mixed, and organic solution is added as solvent, wherein organic
Solution is for dissolving organic siliconresin；Stirring makes biomass waste powder be sufficiently impregnated organic silicones, and then drying is had
The mixture of machine silicones and biomass waste powder；
S03：The mixture of the organic siliconresin obtained in S02 and biomass waste powder is placed in tube furnace, lazy
High temperature sintering under property gas shield, then after keeping the temperature furnace cooling to get SiOC ceramic powders；
S04：It is dry after being performed etching to obtained SiOC ceramic powders using strong base solution；
S05：The SiOC ceramic powders of the S04 dryings walked are placed in tube furnace, are carried out under inert gas protection
Activation heat treatment then takes out after handling in deionized water to neutrality re-dry to get the porous SiOC negative materials of rich carbon.
Further, the preferred bagasse of biomass waste in the S01 steps；In the S01 steps Ball-milling Time be for 24 hours,
Drum's speed of rotation 250r/min.
Further, in the S02 steps organic siliconresin, biomass waste powder and organic solvent mass ratio be (1~
4):(1~3):15.
Further, biomass waste powder is made to be sufficiently impregnated organic silicon tree using heating magnetic agitation in the S02 steps
Fat, the magnetic agitation heating temperature are 50 DEG C, and the magnetic agitation time is 12h, and drying temperature is 75 DEG C, drying time 12h.
Further, high temperature sintering temperature described in the S03 steps is 800~1100 DEG C, and soaking time is 3~5h, whole
Inert gas in a sintering process is Ar, and the inert gas flow amount is 0.1L/min.
Further, sintering process is in the S03 steps：It is 50 DEG C to be sintered initial temperature, is risen to the speed of 5 DEG C/min
400 DEG C, 30min is kept the temperature, then 800~1100 DEG C are warming up to the speed of 5 DEG C/min.
Further, highly basic is KOH solution in the S04 steps, and the solubility of the KOH solution is 10~30%, etching
Time is 3~7h, and drying temperature is 120 DEG C, drying time 12h.
Further, activation heat treatment process described in the S05 steps is：Initial temperature is 50 DEG C, with the speed of 5 DEG C/min
Degree rises to 800 DEG C and keeps the temperature furnace cooling after 2h, and inert gas is Ar, the inert gas flow amount in entire heat treatment process
For 0.1L/min；Drying temperature is 80 DEG C in the S05 steps, drying time 12h.
Further, the rich porous SiOC negative materials ingredient of carbon of the lithium ion battery includes SiOC glass phase and freedom
The microstructure of carbon, the porous SiOC negative materials of the rich carbon of the lithium ion battery is mesoporous and microcellular structure.
Further, the electric discharge for the first time of the porous SiOC negative materials of the rich carbon of the lithium ion battery is 945~1160mAh/
G, the material charge specific capacity are 478~786mAh/g, and coulombic efficiency reaches 53~68% to the material for the first time；The material circulation 60
The reversible specific capacity kept after secondary is 302~628mAh/g.
The beneficial effects of the present invention are：
1. the lithium ion battery of the present invention porous SiOC cathode material preparation methods of rich carbon, pass through organic siliconresin
In contain a large amount of phenyl and saturated hydrocarbons group, cause cracking after SiOC ceramics free carbon content it is higher.
2. the lithium ion battery of the present invention porous SiOC cathode material preparation methods of rich carbon, are carved by potassium hydroxide
It loses and after activation heat treatment, a large amount of mesoporous and micropore can be formed, contribute to buffer lithium ion battery charge and discharge process in this way
In volume change.
3. the lithium ion battery of the present invention porous SiOC negative materials of rich carbon, the free carbon phase of richness not only contributes to it
The improvement of conductivity keeps the non crystalline structure of sample more stable, and sample can be made in Li+Intercalation/deintercalation during show
Lower volume change, so that it is guaranteed that the integrality under the porous SiOC negative materials through a long time charge and discharge cycles of rich carbon.
4. the lithium ion battery of the present invention porous SiOC negative materials of rich carbon, the lithium ion battery are more with rich carbon
The electric discharge for the first time of hole SiOC negative materials is 945~1160mAh/g, which is 478~786mAh/g, the material
Coulombic efficiency reaches 53~68% to material for the first time；The reversible specific capacity kept after the material circulation 60 times is 302~628mAh/g.
Description of the drawings
Fig. 1 is the object phase composition figure of the porous SiOC negative materials of the rich carbon of lithium ion battery in the embodiment of the present invention 8.
Fig. 2 is the cycle performance curve of the porous SiOC negative materials of the rich carbon of lithium ion battery in the embodiment of the present invention 8.
Specific implementation mode
Below in conjunction with the accompanying drawings and specific embodiment the present invention is further illustrated, but protection scope of the present invention is simultaneously
It is without being limited thereto.
A kind of lithium ion battery porous SiOC negative materials of rich carbon and preparation method thereof, include the following steps：
S01：By biomass waste, ball milling, Ball-milling Time are drum's speed of rotation 250r/min for 24 hours after crushing, sieving,
Then take out drying；By treated, biomass waste takes grain size to be less than 64 μm after screening, obtains biomass waste powder.Biology
Matter waste can select bagasse either corn stalk or wheat straw or rice straw.In embodiment for selection bagasse.
S02：Organic siliconresin and bagasse powder are mixed, and organic solution is added as solvent, wherein organic solution
For dissolving organic siliconresin；Organic solution can be dimethylbenzene or tetrahydrofuran；Organic siliconresin, bagasse powder and two
The mass ratio of toluene is (1~4):(1~3):15, heating magnetic agitation 12h makes bagasse powder be sufficiently impregnated at 50 DEG C
Then machine silicones obtains the mixture of organic siliconresin and bagasse powder at 75 DEG C after dry 12h；
S03：The mixture of obtained organic siliconresin and bagasse powder is placed in tube furnace, it is high under Ar gas shieldeds
Temperature sintering, Ar throughputs are 0.1L/min, and sintering initial temperature is 50 DEG C, rise to 400 DEG C with the speed of 5 DEG C/min, heat preservation
30min, then with the speed of 5 DEG C/min be warming up to 800~1100 DEG C heat preservation 3~5h after furnace cooling up to SiOC ceramic powders；
S04：It uses solubility to etch 3~7h to obtained SiOC ceramic powders for 10~30% KOH solution, then exists
Dry 12h at 120 DEG C；
S05：The SiOC ceramic powders of the S04 dryings walked are placed in tube furnace, are activated under Ar gas shieldeds
Heat treatment, Ar throughputs are 0.1L/min, and initial temperature is 50 DEG C, rise to 800 DEG C with the speed of 5 DEG C/min and keep the temperature after 2h with
Furnace cooling but, boils after taking-up, is washed to neutrality in deionized water, and 12h is then dried at 80 DEG C to get the porous SiOC of rich carbon
Negative material.
The beneficial effects of the present invention are using biomass waste material as foraminous die plate, with organic siliconresin it is compound after it is high
The porous SiOC ceramics of the rich carbon of temperature sintering synthesis, recycle etching and activation heat treatment to effectively remove SiO2It is porous that rich carbon is prepared
SiOC negative materials.Lead to the free of the SiOC ceramics after cracking in organic siliconresin containing a large amount of phenyl and saturated hydrocarbons group
Carbon content is higher.Rich free carbon phase present in sample obtained not only contributes to the improvement of its conductivity, makes the amorphous of sample
Structure is more stable, and sample can be made in Li+Intercalation/deintercalation during show lower volume change, so that it is guaranteed that rich
Integrality under the porous SiOC negative materials through a long time charge and discharge cycles of carbon.
The lithium ion battery of the present invention porous SiOC negative materials of rich carbon, the lithium ion battery are porous with rich carbon
SiOC negative material main components include SiOC glass phase and free carbon, the lithium ion battery porous SiOC cathode material of rich carbon
The microstructure of material is mesoporous and microcellular structure.The lithium ion battery is with the electric discharge for the first time of the rich porous SiOC negative materials of carbon
945~1160mAh/g, the material charge specific capacity are 478~786mAh/g, the material for the first time coulombic efficiency reach 53~
68%；The reversible specific capacity kept after the material circulation 60 times is 302~628mAh/g.
Raw material proportioning, process conditions and the parameter that the present invention is respectively implemented are as shown in table 1.
1 embodiment raw material proportioning of table and process conditions
8 embodiments in table 1 are produced into sample, and each embodiment sample to producing according to above-mentioned method
Can test, including BET specific surface area, for the first time electric discharge and charge specific capacity, for the first time coulombic efficiency and cycle 60 times after reversible ratio
Capacity, test result are as shown in table 2.As seen from Table 2, when organic siliconresin content is higher, sintering temperature is higher, soaking time
It is longer, and etch that concentration is higher and when etch period is longer, the porous SiOC negative materials of rich carbon being prepared have higher
Phosphorus content is conducive to the diffusion transport ability for improving lithium ion, and sample has higher specific surface area, forms more nanometer
The good volume change alleviated in charge and discharge process of hole energy, the coulombic efficiency for the first time of sample are improved significantly, cycle 60
Reversible specific capacity after secondary is higher, shows to store up lithium better performances, as described in Example 8.
The performance indicator of the porous SiOC negative materials of the rich carbon of table 2
Fig. 1 is the object phase composition figure of the porous SiOC negative materials of rich carbon prepared in the embodiment of the present invention 8, as seen from the figure sample
Nearby do not occur sharp peak at 24 ° and 44 ° in product, the main broad peak that disperse is presented, mainly due to sample formed it is amorphous
Caused by carbon and SiOC glass phases.
Fig. 2 is the cycle charge-discharge and coulombic efficiency of the porous SiOC negative materials of richness carbon obtained in the embodiment of the present invention 8
Curve graph.The first discharge specific capacity of the product is 1160mAh/g it can be seen from cycle charge-discharge curve, and initial charge can
Inverse specific capacity is 786mAh/g, it is known that the irreversible capacity of product is smaller (374mAh/g), the reversible ratio of charging after recycling 60 times
Capacity is 628mAh/g, illustrates that product has good cyclical stability；Meanwhile it can be with from corresponding coulombic efficiency curve
Find out, the coulombic efficiency for the first time of the product is larger, can reach 68%, and subsequent coulombic efficiency is very high, illustrates the product
Reversibility is preferable.
The embodiment is the preferred embodiments of the present invention, but present invention is not limited to the embodiments described above, not
Away from the present invention substantive content in the case of, those skilled in the art can make it is any it is conspicuously improved, replace
Or modification all belongs to the scope of protection of the present invention.
Claims (10)
1. a kind of lithium ion battery porous SiOC cathode material preparation methods of rich carbon, which is characterized in that include the following steps：
S01：By biomass waste after crushing, sieving ball milling, then take out drying；Will treated biomass waste through sieve
Grain size is taken to be less than 64 μm of biomass waste powder after point；
S02：Organic siliconresin and biomass waste powder are mixed, and organic solution is added as solvent, wherein organic solution
For dissolving organic siliconresin；Stirring makes biomass waste powder be sufficiently impregnated organic silicones, and then drying obtains organosilicon
The mixture of resin and biomass waste powder；
S03：The mixture of the organic siliconresin obtained in S02 and biomass waste powder is placed in tube furnace, in indifferent gas
The lower high temperature sintering of body protection, then after keeping the temperature furnace cooling to get SiOC ceramic powders；
S04：It is dry after being performed etching to obtained SiOC ceramic powders using strong base solution；
S05：The SiOC ceramic powders of the S04 dryings walked are placed in tube furnace, are activated under inert gas protection
Heat treatment then takes out after handling in deionized water to neutrality re-dry to get the porous SiOC negative materials of rich carbon.
2. the lithium ion battery according to claim 1 porous SiOC cathode material preparation methods of rich carbon, which is characterized in that
The preferred bagasse of biomass waste in the S01 steps；Ball-milling Time is drum's speed of rotation 250r/ for 24 hours in the S01 steps
min。
3. the lithium ion battery according to claim 1 porous SiOC cathode material preparation methods of rich carbon, which is characterized in that
The mass ratio of organic siliconresin, biomass waste powder and organic solvent is (1~4) in the S02 steps:(1~3):15.
4. the lithium ion battery according to claim 1 porous SiOC cathode material preparation methods of rich carbon, which is characterized in that
Biomass waste powder is set to be sufficiently impregnated organic silicones, the magnetic agitation using heating magnetic agitation in the S02 steps
Heating temperature is 50 DEG C, and the magnetic agitation time is 12h, and drying temperature is 75 DEG C, drying time 12h.
5. the lithium ion battery according to claim 1 porous SiOC cathode material preparation methods of rich carbon, which is characterized in that
High temperature sintering temperature described in the S03 steps is 800~1100 DEG C, and soaking time is 3~5h, lazy in entire sintering process
Property gas be Ar, the inert gas flow amount be 0.1L/min.
6. the lithium ion battery according to claim 1 porous SiOC cathode material preparation methods of rich carbon, which is characterized in that
Sintering process is in the S03 steps：It is 50 DEG C to be sintered initial temperature, rises to 400 DEG C with the speed of 5 DEG C/min, heat preservation
30min, then it is warming up to 800~1100 DEG C with the speed of 5 DEG C/min.
7. the lithium ion battery according to claim 1 porous SiOC cathode material preparation methods of rich carbon, which is characterized in that
Highly basic is KOH solution in the S04 steps, and the solubility of the KOH solution is 10~30%, and etch period is 3~7h, dry
Temperature is 120 DEG C, drying time 12h.
8. the lithium ion battery according to claim 1 porous SiOC cathode material preparation methods of rich carbon, which is characterized in that
Activation heat treatment process is described in the S05 steps：Initial temperature is 50 DEG C, rises to 800 DEG C with the speed of 5 DEG C/min and protects
Furnace cooling after warm 2h, inert gas is Ar in entire heat treatment process, and the inert gas flow amount is 0.1L/min；It is described
Drying temperature is 80 DEG C in S05 steps, drying time 12h.
9. a kind of utilizing the porous SiOC negative materials of rich carbon of lithium ion battery made from preparation method described in claim 1,
It is characterized in that, the rich porous SiOC negative materials ingredient of carbon of the lithium ion battery includes SiOC glass phase and free carbon, described
The microstructure of the porous SiOC negative materials of lithium ion battery richness carbon is mesoporous and microcellular structure.
10. the lithium ion battery according to claim 9 porous SiOC negative materials of rich carbon, which is characterized in that the lithium
The electric discharge for the first time of the porous SiOC negative materials of ion battery richness carbon is 945~1160mAh/g, which is
478~786mAh/g, coulombic efficiency reaches 53~68% to the material for the first time；The reversible specific capacity kept after the material circulation 60 times
For 302~628mAh/g.
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| CN113248257A (en) * | 2021-05-12 | 2021-08-13 | 浙江大学 | Co-continuous macroporous SiOC negative electrode material of lithium ion battery and preparation method thereof |
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| CN114057488A (en) * | 2022-01-17 | 2022-02-18 | 河南科技学院 | Preparation method of porous SiOC ceramic and application of porous SiOC ceramic in negative electrode material of lithium ion battery |
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| 潘建梅等: ""前驱体热解制备多孔SiOC复合材料及性能"", 《硅酸盐学报》 * |
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| CN114122376A (en) * | 2021-11-12 | 2022-03-01 | 宁德新能源科技有限公司 | Electrochemical device and electronic device comprising same |
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