CN107623104A - A kind of structure silicon-based negative material of multi-buffer and preparation method thereof - Google Patents
A kind of structure silicon-based negative material of multi-buffer and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to structure silicon-based negative material of a kind of multi-buffer and preparation method thereof, belong to materials processing technology field.The present invention is by nano silica fume Surface coating nanometer titanium dioxide layer, the cushion of silicon particle Volume Changes during by the use of the rock-steady structure of nano titanium oxide as embedding de- lithium, successfully inhibit the polymerization and peeling of silicon particle, and improve the chemical property of electrode material, amorphous carbon layer is coated again, prepare the silicon based electrode material of double-coating structure, the volumetric expansion of activated silica kernel has effectively been buffered in charge and discharge process by two-coat, maintain the stability of electrode/electrolyte interface and surface SEI films, so that composite shows good cycle performance.
Description
Technical field
The present invention relates to structure silicon-based negative material of a kind of multi-buffer and preparation method thereof, belongs to materials processing technology neck
Domain.
Background technology
Coal, natural gas, oil etc. are the larger traditional energies of current application amount, promote the hair of industry and entire society
Exhibition.But with the rapid development of economy, the mankind increase the consumption to fossil fuel, the problem of causing environmental pollution, further dislikes
Change, oneself is through seriously affecting the existence of the mankind.Fossil fuel is the energy substance based on carbon, a large amount of combustions of fossil fuel
Burning will certainly produce substantial amounts of carbon dioxide, and carbon dioxide will lift global temperatures, cause sea level as greenhouse gases
Rise, Changes in weather is variable, and the movable scope of the mankind gradually decreases.And other elements in fossil fuel, such as N, S etc., they
The water droplet that a part can be generated in acidic oxide, with air combines to form acid rain, corrosion building, acidified soil, harm agricultural；
Another part forms aerosol systems, and its a large amount of aggregation has reformed into haze, influences ecological environment, endangers human physical and mental health.For
Influenceed caused by alleviation environmental pollution, the mankind have to reduce the utilization rate of fossil fuel, and sight is transferred into cleaning energy
On source.Clean energy resource refers to the energy not discharged pollutants.In addition to nuclear energy, mainly including hydroelectric generation, wind-power electricity generation, the sun
The regenerative resources such as energy, biogas, but these energy need large-scale converting apparatus mostly, and affected by environment big, using energy source
Rate is low.And lithium ion battery has the advantages that big energy density, long lifespan, small volume and less weight, not only existed as one of clean energy resource
Microminiature appliance field has been used widely, and with power system of electric automobile and intelligent grid energy storage device etc.
The application development for the equipment that maximizes, by as one of current research and application clean energy resource of greatest concern.
Several years, country supported the development of new-energy automobile energetically, and lithium ion battery also will be therewith towards high power, high energy
Amount, the direction in high circulation life-span continue to develop.Lithium ion battery mainly by positive pole, barrier film, negative pole, organic electrolyte, battery outside
Shell forms.The wherein shared value of positive pole, negative pole, barrier film, organic electrolyte is bigger, is the core component of lithium ion battery.
Early stage, negative material of the lithium usually as lithium ion battery are studied in negative material.In charge and discharge process,
Lithium can reach certain specific capacity, but the lithium ion returned from positive pole can form Li dendrite in lithium piece surface sediment, pierce through every
Film, cause battery short circuit, even explode.So lithium makees metal negative electrode, potential safety hazard is very big.In order to solve this problem, permitted
The alternative materials of lithium metal are all found in more researchs.Main research range is carbons material, metal and metallic compound.Due to lithium from
Son be able to will be embedded in negative material, and keeps a stable state, so to become security best for carbons negative material
Negative material.The electrochemical reaction of carbons material and lithium ion is close to lithium metal, and lithium is in negative pole deintercalation, the crystalline substance of carbons material
Body structure can keep stable, and the lithium ion battery for doing negative pole with carbons material has good recycling performance, still, now
The negative material graphite material used, since lithium ion battery is commercialized, actual discharge specific capacity is own to pass through close to 372mAh/g
Theoretical value, turn into restrict lithium battery continue development bottleneck, finding the novel anode material of height ratio capacity turns into current negative pole
Investigation of materials emphasis.
Silicium cathode material has a specific discharge capacity of superelevation, alternative carbons material, improves the electric discharge ratio of carbon negative pole material
Capacity, still, silicon is in process of intercalation, it may occur that huge Volume Changes, heavy damage electrode is stable, and silicon is semiconductor
Material, its electric conductivity is poor, and the cycle life of silicon materials is poor, and first charge-discharge efficiency is relatively low, and complicated preparation technology makes
Many influence factors are difficult to control, and cause material property unstable.
So negative material affects the performance of lithium ion battery.In order that being optimal of performance of lithium ion battery, bears
Pole material should meet following condition：
(1) negative material potential is as low as possible, and larger electrical potential difference is formed with positive electrode.Influence of electric potential the electrification in battery
Reaction is learned, so the potential of negative material should level off to the electrochemical potential of lithium；
(2) material structure is stable, and when embedded and deintercalation occurs for negative pole, material crystal structure can not occur significantly to become lithium ion
Change；
(3) material has higher lithium ion diffusion coefficient；
(4) material has higher ionic conductivity；
(5) material density is suitable, has higher electrode density.
The content of the invention
The technical problems to be solved by the invention：For silicon in process of intercalation, huge Volume Changes occur, it is serious broken
Bad electrode is stable, and electric conductivity is poor, and the cycle life of composite is poor, and first charge-discharge efficiency is relatively low, complicated
Preparation technology is difficult to control many influence factors, the problem of causing material property unstable, there is provided a kind of multi-buffer knot
Structure silicon based anode material and preparation method thereof.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
By nano silica fume Surface coating nanometer titanium dioxide layer, then coat amorphous carbon layer and be made.
The nano silica fume is that 325 mesh sieve micron silicons, 10~12h of ball milling under argon atmosphere is made.
The cladding nanometer titanium dioxide layer is in butyl titanate and the Compound Water of ethanol by nano silica fume ultrasonic disperse
It is spray-dried to be made in solution.
The mol ratio of the nano silica fume and butyl titanate is 1：4.
The spray drying EAT is 250~270 DEG C, and leaving air temp is 110~120 DEG C.
The cladding amorphous carbon layer be by coated by titanium dioxide silicon ultrasonic disperse in sucrose ethanol solution, then 80~
It is evaporated to dryness and is placed in tube furnace at 90 DEG C, grinds and be made after insulation reaction.
The mass ratio of the sucrose and coated by titanium dioxide silicon is 3：7.
The insulation reaction is under argon atmosphere, is warming up to 400~500 DEG C with 5~10 DEG C/min heating rates, insulation
700~800 DEG C are warming up to 5~10 DEG C/min heating rates after 2~3h of reaction, 2~3h of insulation reaction.
Concretely comprise the following steps：
S1. by micron silicon under argon atmosphere 10~12h of ball milling, obtain nano silica fume；
S2. it is to be well mixed in 80% ethanol solution to take butyl titanate to add mass fraction, adds nano silica fume, ultrasound point
It is fitted into after scattered 30~40min in spray dryer and is spray-dried, obtains coated by titanium dioxide silicon；
S3. coated by titanium dioxide silicon is taken to add in sucrose/ethanol solution, 20~30min of ultrasonic disperse, then it is transferred to Rotary Evaporators
In, it is evaporated to dryness at 80~90 DEG C, obtains precursor；
S4. precursor is placed in tube furnace, 3~5h of grinding in mortar is fitted under argon atmosphere, after insulation reaction, is obtained multiple
Buffer structure silicon based anode material.
Compared with other method, advantageous effects are the present invention：
The present invention by nano silica fume Surface coating nanometer titanium dioxide layer, by the use of nano titanium oxide rock-steady structure as
The cushion of silicon particle Volume Changes during embedding de- lithium, successfully inhibits the polymerization and peeling of silicon particle, and improves electricity
The chemical property of pole material, then amorphous carbon layer is coated, the silicon based electrode material of double-coating structure is prepared, is covered by double-contracting
Layer has effectively buffered the volumetric expansion of activated silica kernel in charge and discharge process, maintains electrode/electrolyte interface and surface SEI
The stability of film so that composite shows good cycle performance.
Embodiment
Take 5~10g325 mesh sieves micron silicon to add in stainless steel jar mill, 10~12h of ball milling under argon atmosphere, must receive
Rice silica flour, it is in 80% ethanol solution, with 300~400r/ to take 34~68g butyl titanates to add 300~600mL mass fractions
Min stirs 10~15min, adds 2.8~5.6g nano silica fumes, loads after disperseing 30~40min with 300W ultrasonic echographies
It is spray-dried in spray dryer, it is 250~270 DEG C to control EAT, and leaving air temp is 110~120 DEG C, obtains titanium dioxide
Coated Si, takes 3.5~7.0g coated by titanium dioxide silicon, adds 150~300g mass fractions and is in 1% sucrose/ethanol solution, with
300W ultrasonic echographies disperse 20~30min, then are transferred in Rotary Evaporators, are evaporated to dryness at 80~90 DEG C, obtain precursor,
Precursor is placed in tube furnace, under argon atmosphere, is warming up to 400~500 DEG C with 5~10 DEG C/min heating rates, insulation
700~800 DEG C are warming up to 5~10 DEG C/min heating rates after 2~3h of reaction, 2~3h of insulation reaction, is filled after being cooled to room temperature
Enter 3~5h of grinding in mortar, obtain multiple buffer structure silicon based anode material.
Example 1
5g325 mesh sieves micron silicon is taken to add in stainless steel jar mill, ball milling 10h, obtains nano silica fume under argon atmosphere,
It is in 80% ethanol solution to take 34g butyl titanates to add 300mL mass fractions, stirs 10min with 300r/min, then add
Enter 2.8g nano silica fumes, disperse after 30min to be fitted into spray dryer to be spray-dried with 300W ultrasonic echographies, control into wind-warm syndrome
Spend for 250 DEG C, leaving air temp is 110 DEG C, obtains coated by titanium dioxide silicon, takes 3.5g coated by titanium dioxide silicon, adds 150g mass
Fraction is in 1% sucrose/ethanol solution, disperses 20min with 300W ultrasonic echographies, then is transferred in Rotary Evaporators, at 80 DEG C
It is evaporated to dryness, obtains precursor, precursor is placed in tube furnace, under argon atmosphere, is warming up to 5 DEG C/min heating rates
400 DEG C, 700 DEG C, insulation reaction 2h are warming up to 5 DEG C/min heating rates after insulation reaction 2h, are cooled to after room temperature to load and are ground
3h is ground in alms bowl, obtains multiple buffer structure silicon based anode material.
Example 2
8g325 mesh sieves micron silicon is taken to add in stainless steel jar mill, ball milling 11h, obtains nano silica fume under argon atmosphere, takes 51g
It is in 80% ethanol solution that butyl titanate, which adds 450mL mass fractions, stirs 12min with 350r/min, adds 4.2g nanometers
Silica flour, disperse after 35min to be fitted into spray dryer to be spray-dried with 300W ultrasonic echographies, it is 260 DEG C to control EAT,
Leaving air temp is 115 DEG C, obtains coated by titanium dioxide silicon, takes 5g coated by titanium dioxide silicon, add 280g mass fractions be 1% sucrose/
In ethanol solution, 25min is disperseed with 300W ultrasonic echographies, then is transferred in Rotary Evaporators, is evaporated to dryness at 85 DEG C, before obtaining
Body, precursor is placed in tube furnace, under argon atmosphere, is warming up to 450 DEG C with 8 DEG C/min heating rates, insulation reaction
750 DEG C, insulation reaction 2h are warming up to 8 DEG C/min heating rates after 2h, is cooled to after room temperature to be fitted into mortar and grinds 4h, much
Weight buffer structure silicon based anode material.
Example 3
10g325 mesh sieves micron silicon is taken to add in stainless steel jar mill, ball milling 12h, obtains nano silica fume under argon atmosphere, takes 68g
It is in 80% ethanol solution that butyl titanate, which adds 600mL mass fractions, stirs 15min with 400r/min, adds 5.6g nanometers
Silica flour, disperse after 40min to be fitted into spray dryer to be spray-dried with 300W ultrasonic echographies, it is 270 DEG C to control EAT,
Leaving air temp is 120 DEG C, obtains coated by titanium dioxide silicon, takes 7.0g coated by titanium dioxide silicon, and it is 1% sugarcane to add 300g mass fractions
In sugar/ethanol solution, 30min is disperseed with 300W ultrasonic echographies, then is transferred in Rotary Evaporators, is evaporated to dryness at 90 DEG C,
Precursor is obtained, precursor is placed in tube furnace, under argon atmosphere, is warming up to 500 DEG C with 10 DEG C/min heating rates, insulation
With 10 DEG C/min heating rates 800 DEG C, insulation reaction 3h are warming up to after reaction 3h, are cooled to after room temperature to be fitted into mortar and grind
5h, obtain multiple buffer structure silicon based anode material.
The first charge-discharge capacity of silicon-carbon composite cathode material is respectively 500.2mAh/g, 648.1mAh/g after tested, first
Secondary efficiency for charge-discharge can reach 77.2%.Composite has higher reversible capacity, mainly due in process of intercalation,
The film forming area of SEI films is reduced, and the consumption of lithium ion is reduced therewith;During de- lithium, graphite is led with what amorphous carbon was formed
Electric network ensure that the electrical contact of silicon grain, and silicon grain will not depart from because of bulk effect and collector, cause Li+It can not take off
Go out, form dead lithium, so as to cause the loss of reversible capacity.In subsequent the 2nd time and the 3rd cyclic process, discharge curve base
This is consistent, does not have a greater change, shows that the SEI films that material is formed in process of intercalation first are relatively stable, not follow-up
New irreversible capacity is produced in cyclic process, is delayed well so the addition of graphite serves to the bulk effect of silicon removal lithium embedded
Punching acts on.
In the charge and discharge process of early stage, because the passage of Lithium-ion embeding negative material is not opened completely, cause portion
Point active material has neither part nor lot in reaction, and occur that material discharging specific capacity is stepped up before place in the cyclic process of 15 weeks shows
As.The coulombic efficiency of material reaches more than 97%, after circulating 30 weeks, discharge capacity 528mAh/g, has good cyclicity
Energy.This is primarily due to amorphous carbon and graphite has buffered the bulk effect of silicon removal lithium embedded, restrained effectively material SEI films
It is continuously generated, reduces Li+Loss in cyclic process.In addition, amorphous carbon coating layer adds the combination of graphite and silicon
Power, the quick efflorescence of material is avoided, so as to improve the cyclical stability of material.
Claims (9)
1. a kind of structure silicon-based negative material of multi-buffer, it is characterised in that it is by nano silica fume Surface coating nanometer two
Titanium oxide layer, then coat amorphous carbon layer and be made.
2. a kind of structure silicon-based negative material of multi-buffer as claimed in claim 1, it is characterised in that the nano silica fume is
325 mesh sieve micron silicons, 10~12h of ball milling under argon atmosphere is made.
A kind of 3. structure silicon-based negative material of multi-buffer as claimed in claim 1, it is characterised in that the cladding nanometer two
Titanium oxide layer be by nano silica fume ultrasonic disperse in the compound aqueous solution of butyl titanate and ethanol, it is spray-dried to be made.
A kind of 4. structure silicon-based negative material of multi-buffer as claimed in claim 3, it is characterised in that the nano silica fume with
The mol ratio of butyl titanate is 1：4.
A kind of 5. structure silicon-based negative material of multi-buffer as claimed in claim 3, it is characterised in that it is described be spray-dried into
Air temperature is 250~270 DEG C, and leaving air temp is 110~120 DEG C.
6. a kind of structure silicon-based negative material of multi-buffer as claimed in claim 1, it is characterised in that the cladding is amorphous
Carbon-coating be by coated by titanium dioxide silicon ultrasonic disperse in sucrose ethanol solution, then be evaporated to dryness at 80~90 DEG C and be placed in pipe
Grind and be made in formula stove, after insulation reaction.
7. a kind of structure silicon-based negative material of multi-buffer as claimed in claim 5, it is characterised in that the sucrose and dioxy
The mass ratio for changing titanium coated Si is 3：7.
8. a kind of structure silicon-based negative material of multi-buffer as claimed in claim 5, it is characterised in that the insulation reaction is
Under argon atmosphere, 400~500 DEG C are warming up to 5~10 DEG C/min heating rates, after 2~3h of insulation reaction with 5~10 DEG C/
Min heating rates are warming up to 700~800 DEG C, 2~3h of insulation reaction.
9. a kind of preparation method of the structure silicon-based negative material of multi-buffer as described in claim 1~8 any one, it is special
Sign is, concretely comprises the following steps：
S1. by micron silicon under argon atmosphere 10~12h of ball milling, obtain nano silica fume；
S2. it is to be well mixed in 80% ethanol solution to take butyl titanate to add mass fraction, adds nano silica fume, ultrasound point
It is fitted into after scattered 30~40min in spray dryer and is spray-dried, obtains coated by titanium dioxide silicon；
S3. coated by titanium dioxide silicon is taken to add in sucrose/ethanol solution, 20~30min of ultrasonic disperse, then it is transferred to Rotary Evaporators
In, it is evaporated to dryness at 80~90 DEG C, obtains precursor；
S4. precursor is placed in tube furnace, 3~5h of grinding in mortar is fitted under argon atmosphere, after insulation reaction, is obtained multiple
Buffer structure silicon based anode material.
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| CN108520955A (en) * | 2018-06-07 | 2018-09-11 | 成都硅宝科技股份有限公司 | Three-dimensional net structure nano-silicone wire/carbon/titanium oxide composite material and preparation method |
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| CN112366306B (en) * | 2021-01-12 | 2021-04-09 | 拓米(成都)应用技术研究院有限公司 | Nano silicon composite negative electrode material and manufacturing method thereof |
| CN113036135A (en) * | 2021-02-26 | 2021-06-25 | 昆山宝创新能源科技有限公司 | Composite negative electrode material, preparation method thereof, pole piece, battery and device |
| CN113036137A (en) * | 2021-03-05 | 2021-06-25 | 昆山宝创新能源科技有限公司 | Lithium ion battery cathode material and preparation method and application thereof |
| CN114132914A (en) * | 2021-11-25 | 2022-03-04 | 广东凯金新能源科技股份有限公司 | Titanium dioxide-carbon double-layer coated silicon-based composite material, and preparation method and application thereof |
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