CN109755519A - A kind of Anode of lithium cell material and preparation method thereof with ductility carbon material cladding - Google Patents
A kind of Anode of lithium cell material and preparation method thereof with ductility carbon material cladding Download PDFInfo
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Abstract
The present invention provides a kind of Anode of lithium cell materials and preparation method thereof with ductility carbon material cladding, using one or more small organic molecules containing two or more element in C, H, O, N, and the organic matter contains N element and has cyclic structure, under suitable catalyst and thermodynamic condition, one layer of Anode of lithium cell material coated using ductility carbon material as shell is cracked to form on anode material powder surface.Gained Anode of lithium cell material have inorganic extending clad, cladding carbon content between 0.5%-10%, cladding after material particle size in D50It is 4.5-11.5 μm, specific surface area is 8-18 m2/g.The present invention solves the ductility problem of active material surface clad, improves the cycle performance of anode material.
Description
Technical field
The present invention relates to Anode of lithium cell material and preparation method thereof more particularly to it is a kind of with ductility carbon material cladding
Lithium ion battery anode material and preparation method thereof.
Background technique
Due to the limitation of current material system, the energy density of commercialization rocking chair type lithium ion battery and battery pack is
Reach bottleneck.In order to promote the energy density of commercialized lithium ion battery and its battery pack, meet the requirement of market and application,
High-capacity anode material is one of the important development direction of the following lithium ion battery anode material.However the lithium-ion electric of high capacity
Pond anode material such as silicon, tin and its alloy or oxide and some metal oxides all exist and lead because volume expansion is excessive
The problem of causing SEI membrane interface unstable and generating repeatedly causes the rapid decay of chemical property.Current mainstream processing method
It is to carry out primary cladding processing on the cationic materials surface of high capacity, the mode that even ghost reserves expansion space improves.
But still remain more problem.
Such as CN103531760, although prepared by the hollow egg shell-core structure of porous carbon can be interior nuclear active material
Expansion reserved space.But structure is easily destroyed the material in the actual processing process, and complex process, and sour dosage is big, and
Clad is that porous carbon is difficult intact isolation electrolyte.Therefore actually elevating from practicability and performance, Shang You
Defect.
Based on this, a kind of lithium ion of the Promethean inorganic extending carbon material cladding for being prepared for core-shell structure of this patent
Battery anode material, the material can be by with one or more small points containing two or more element in C, H, O, N
(this kind of organic matter also needs itself have certain cyclic structure can to sub- organic matter (wherein at least one organic matter contains N element)
Think coordination ring, pyridine ring, phenyl ring etc.) it is carbon source, it gives suitable catalyst and thermodynamic condition can be in lithium ion battery
The powder surface of anode material is cracked to form one layer of anode of lithium ion battery material to curl and extending carbon material is coated as shell
Material.
Summary of the invention
The present invention is for overcome the deficiencies in the prior art, to provide a kind of core coated using inorganic extending carbon material as shell
Shell structure lithium ion battery anode material and preparation method thereof.
The present invention is achieved by the following technical programs:
A kind of preparation method of the Anode of lithium cell material with ductility carbon material cladding, comprising the following steps:
A1, carbon source, the powder core for making anode of lithium ion battery, catalyst are placed in reactor, then are passed through inert gas
Displaced air atmosphere, and by pressure control in 1atm-5atm.
A2, after stable gas pressure and oxygen content is lower than after 200ppm, reactor is warming up to 500-1200 DEG C of temperature range
It is interior, carry out catalytic pyrolysis 1-8h.
A3, heat is carried out in 700-1200 DEG C of temperature range after the completion of catalytic pyrolysis, then by temperature of reactor control
Handle 1-8h.
A4,65 DEG C are subsequently cooled to hereinafter, pressure release and go inertia except protective atmosphere, obtain coating with ductility carbon material
Lithium ion battery anode material with core-shell structure.
Further, in step A1, the carbon source be one kind containing two or more element in C, H, O, N or
A variety of small organic molecules, the small organic molecule contains N element and molecular structure has cyclic structure.
Preferably, the carbon source includes but is not limited to heterocyclic compound, pyridines, miazines, the complexing containing phenyl ring and nitrogen
Object, the object that spreads out of benzene, amide derivatives, heteroaromatic hydrocarbon.
Further, in step A1, it is described be used to make anode of lithium ion battery powder core be rocking chair type lithium from
Pass through the active material particle with volume expansion in removal lithium embedded progress charge and discharge process in sub- battery system.
Preferably, the powder core for being used to make anode of lithium ion battery includes but is not limited to the list of the IVth major element
Matter and its derivative, the simple substance and its derivative of transition metal element.
Preferably, it is described be used to make anode of lithium ion battery powder core be Si, Sn, C simple substance or its oxide, and
Using nano-silicon as function reinforced phase, hard carbon or soft carbon are the micron composite particles of matrix preparation.
Further, in step A1, the carbon source and catalyst are placed in reactor in the form of solid phase or liquid phase, or
Carbon source and catalyst are gasified, and mixed inert gas is passed through in reactor and carries out cracking deposition.
Further, in step A2, the heating at the uniform velocity heating or it is non-at the uniform velocity heat up, or set in temperature-rise period
Set moderate soak link, but average heating rate should control 0.2 DEG C per minute to 20 DEG C per minute between.
Preferably, the inert gas includes nitrogen, argon gas or its mixed gas, and the per minute of the inert gas leads to
Tolerance is not more than the 20% of reactor total volume, preferably 0.1%-10%.
Preferably, the air pressure is constant pressure or pulsed air pressure, and when using pulsed air pressure, the pressure of the air pressure is taken
The pressure difference of intermediate value air pressure, limiting pressure and intermediate value air pressure is not more than ± the 30% of intermediate value air pressure.
Further, the catalyst is one of molybdenum, copper, nickel, iron, cobalt, chromium, platinum, titanium, calcium halophosphate activated by antimony andmanganese, aluminium, silicon simple substance
Or alloy, covalent compound, complex, complex compound or the cyclopentadienyl compounds of a variety of simple substance.
Further, the mass fraction of the catalyst is not more than 10%, preferably 0.05%-5.5%.
A kind of Anode of lithium cell material coated with ductility carbon material, which is characterized in that the Anode of lithium cell material
It is to be prepared according to a kind of preparation method of above-mentioned Anode of lithium cell material with ductility carbon material cladding.
Further, the Anode of lithium cell material has core-shell structure；Wherein, shell structure is ductility carbon material cladding
Layer, the class graphite carbon-coating that the ductility carbon material clad is adulterated by several layers of N are constituted；Nuclear structure is in rocking chair type lithium-ion electric
Pass through the active material particle with volume expansion in removal lithium embedded progress charge and discharge process in pond body system.
Further, a kind of Anode of lithium cell material coated with ductility carbon material, it is characterised in that:
(I) the Anode of lithium cell material has core-shell structure, wherein shell structure is ductility carbon material clad, described to prolong
The class graphite carbon-coating that malleability carbon material clad is adulterated by several layers of N is constituted；
(II) the Anode of lithium cell material has ductility, and the ductility derives from the M type that fold is crimped with multilayer carbon
The ductility carbon material clad that the form of superposition is constituted, the ductility carbon material clad have the multilayer carbon for curling of extending
Nanometer wall array structure；
(III) the Anode of lithium cell material has core-shell structure, wherein nuclear structure is in rocking chair type lithium-ion battery system
The active material particle that volume expansion is had in charge and discharge process is carried out by removal lithium embedded.
(IV) outer surface of the Anode of lithium cell material is enclosed with ductility carbon material clad, the ductility carbon materials
The inorganic carbon content of material clad is between 0.5%-10%, the granularity D of the Anode of lithium cell material50It is 4.5-11.5 μm, vibration
Real density is 0.4-1.4 g/cm3, specific surface area is 8-18 m2/g；The reversible capacity 700 of the Anode of lithium cell material ~
68 ~ 92%, 600 weeks 1450mAh/g, first effect circulation conservation rates are greater than 93%.
Compared with prior art, the present invention is had the advantages that
Experiment discovery, by rationally controlling the condition of nitrogen-doping and catalysis, can make N element to be graphitized N or pyridine N
Form be doped into graphite linings, in view of multi-layer graphene monocrystalline itself be easy for because intermolecular Van der Waals force generate fold, no
Destroy carbon-coating.The incorporation of N element changes sp between original fixed C-C2The structure of hydridization formation hexaplanar；It is mixing simultaneously
Because its polyelectron and the mainly presence in the form of σ key of C-N key, induce so that the C-C key between carbon-coating also occurs in miscellaneous process
The σ key of sp hydridization.There is angle bending so as to cause the plane carbon-coating for itself shoulding be hexaplanar grid.When by reacting item
When part carries out control appropriate to doping, it can be formed outside powder material particles core continuous and uniformly there is this kind of special volume
The bent extending film of multilayer carbon nanowalls obtains the Anode of lithium cell material coated with ductility carbon material.
The method of the present invention passes through controllable cracking, and one layer of inorganic extending carbon material packet can be formed outside active material particle
Coating, with the expansion of active material particle matrix, has the M type stacking pattern of curling fold in lithium ion telescopiny
Clad be drawn as the state of opposing straight, cladding layer film basic structure keeps good, thus allow clad with
In active substance expansion and extend；During material takes off lithium, clad again can be with the receipts of interior active substance
It contracts and retracts, form stable interface with electrolyte, guarantee the relatively stable of SEI film.The method of the present invention preparation with ductility
The Anode of lithium cell material of carbon material cladding, since clad has ductility, in the premise with preferable electronic conductivity
Under, the expansion of matrix can be also endured, existing Anode of lithium cell material core-shell structure is unstable, it is swollen to be easy to well solve
The poor problem of swollen damage, cycle performance.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the clad of the Anode of lithium cell material coated with ductility carbon material.
Fig. 2 is the TEM figure of the Anode of lithium cell material with ductility carbon material cladding of the method for the present invention preparation.
Fig. 3 is the height after the removal lithium embedded of the Anode of lithium cell material with ductility carbon material cladding of the method for the present invention preparation
Times SEM figure.
Specific embodiment
Embodiment 1
A kind of preparation method of the Anode of lithium cell material with ductility carbon material cladding of 1#, steps are as follows:
(I) it using benzene and acetamide as raw material, is mixed after flashing to gas with volume ratio 1:1, is then diluted to 30% body with nitrogen
Fraction forms mixed gas；
(II) 500g commercialization SiO micron particles, Cu 3g are respectively implanted in reactor, are controlled reactor with nitrogen atmosphere
In 1.2atm constant pressure, oxygen content is lower than 200ppm；
(III) continue to lead to nitrogen with the ventilatory capacity of 80ml/min, pressure is maintained at 1.2atm, and with the heating of 10 DEG C/min speed
Reactor is warming up to 500 DEG C by rate；
(IV) when temperature rises to 500 DEG C, gas is switched to the mixed gas in step (I), will be mixed with 1L/min speed
Gas is passed through reactor, and is warming up to 900 DEG C with 5 DEG C of rates per minute and keeps the temperature 2 hours；
(V) gas is switched to nitrogen, is continuously heating to 1100 DEG C and keeps the temperature 3 hours；
(VI) it is switched to nitrogen after reaction to continue to lead to nitrogen with the ventilatory capacity of 80ml/min, pressure is maintained at 1.2atm certainly
65 DEG C of pressure releases are so cooled to, sieving can obtain the SiO material coated with ductility carbon material.
The theoretical construct schematic diagram of the SiO material of the ductility carbon material cladding is as shown in Figure 1；The ductility carbon materials
Expect that the TEM figure of the SiO material of cladding is as shown in Figure 2；High power of the SiO material of the ductility carbon material cladding after removal lithium embedded
SEM figure is as shown in Figure 3.
Embodiment 2
A kind of preparation method of the Anode of lithium cell material with ductility carbon material cladding of 2#, steps are as follows:
(I) it using toluene and amino-formaldehyde as raw material, is mixed after flashing to gas with volume ratio 1:1, is then diluted to nitrogen
30% volume fraction forms mixed gas；
(II) by the commercially available SnO of 500g2(wherein ,-x micron particles, cupric tetramminosulfate (II) 3g are respectively put into reaction cavity
SnO2- x micron particles, cupric ammine complex mass ratio be how many, cupric ammine complex writes out specific molecular formula), with nitrogen atmosphere
By reactor control in 1.5atm constant pressure, oxygen content is lower than 200ppm；
(III) continue to lead to nitrogen with the ventilatory capacity of 80ml/min, pressure is maintained at 1.2atm, and with the heating of 10 DEG C/min speed
Reactor is warming up to 500 DEG C by rate；
(IV) when temperature rises to 500 DEG C, gas is switched to the mixed gas in step (I), will be mixed with 1L/min speed
Gas is passed through reactor, and is warming up to 850 DEG C with 5 DEG C of rates per minute and keeps the temperature 5 hours；
(V) it is switched to nitrogen after reaction to continue to lead to nitrogen with the ventilatory capacity of 80ml/min, pressure is maintained at 1.4atm certainly
65 DEG C of pressure releases are so cooled to, sieving can obtain the SnO coated using inorganic extending carbon material as shell2- x material.
Embodiment 3
A kind of preparation method of the Anode of lithium cell material with ductility carbon material cladding of 3#, steps are as follows:
(I) it using benzene and acetamide as raw material, is mixed after flashing to gas with volume ratio 1:1, is then diluted to 30% body with nitrogen
Fraction forms mixed gas；
(II) 500g is commercialized Nano-Si-C composite micron particles, Valine copper complex is respectively put into reaction
Cavity is controlled reactor in 1.2atm constant pressure with nitrogen atmosphere, and oxygen content is lower than 200ppm；
(III) continue to lead to nitrogen with the ventilatory capacity of 80ml/min, pressure is maintained at 1.2atm, and with the heating of 10 DEG C/min speed
Reactor is warming up to 500 DEG C by rate；
(IV) when temperature rises to 500 DEG C, gas is switched to the mixed gas in step (I), will be mixed with 1L/min speed
Gas is passed through reactor, and is warming up to 850 DEG C with 5 DEG C of rates per minute and keeps the temperature 2 hours；
(VI) it is switched to nitrogen after reaction to continue to lead to nitrogen with the ventilatory capacity of 80ml/min, pressure is maintained at 1.2atm certainly
35 DEG C of pressure releases are so cooled to, sieving can obtain the Nano-Si-C composite coated using inorganic extending carbon material as shell
Material.
Embodiment 4
A kind of preparation method of the Anode of lithium cell material with ductility carbon material cladding of 4#, steps are as follows:
(I) with phenylamino and methylpyrrole mixing for standby use；
(II) 500g is commercialized Nano-Si-C composite micron particles, Valine copper complex is respectively put into reaction
Cavity is controlled reactor in 1.2atm constant pressure with nitrogen atmosphere, and oxygen content is lower than 200ppm；
(III) continue to lead to nitrogen with the ventilatory capacity of 80ml/min, pressure is maintained at 1.2atm, and with the heating of 10 DEG C/min speed
Reactor is warming up to 500 DEG C by rate；
(IV) when temperature rises to 500 DEG C, the mixing liquid of (I) is passed through reaction cavity with 1ml/min, pressure control is in 0.7-
The pulse of 1.3atm, low pressure high pressure constant voltage time be 10 minutes, boost process be 30 seconds, control pressure and with 5 DEG C per minute
Rate be warming up to 850 DEG C keep the temperature 2 hours；
(VI) it is switched to nitrogen after reaction to continue to lead to nitrogen with the ventilatory capacity of 80ml/min, pressure is maintained at 1.2atm certainly
35 DEG C of pressure releases are so cooled to, sieving can obtain the Nano-Si-C composite coated using inorganic extending carbon material as shell
Material.
Embodiment 5
A kind of preparation method of the Anode of lithium cell material with ductility carbon material cladding of 5#, steps are as follows:
(I) 500g SiO micron particles, Cu 3g, polyphenyl acetonitrile 20g is commercialized to be respectively implanted in reactor, it will with nitrogen atmosphere
Reactor control is lower than 200ppm in 1.2atm constant pressure, oxygen content；
(II) continue to lead to nitrogen with the ventilatory capacity of 80ml/min, pressure is maintained at 1.2atm, and with the heating rate of 3 DEG C/min
Reactor is warming up to 250 DEG C；
(III) reactor is warming up to 500 DEG C with the heating rate of 8 DEG C/min, keeps the temperature 3 hours.
(IV) when temperature rises to 500 DEG C, gas is switched to argon gas, argon gas is passed through by reaction with 1L/min speed
Device, and be warming up to 900 DEG C with 5 DEG C of rates per minute and keep the temperature 2 hours；
(V) gas is switched to nitrogen, is continuously heating to 1100 DEG C and keeps the temperature 3 hours；
(VI) it is switched to nitrogen after reaction to continue to lead to nitrogen with the ventilatory capacity of 80ml/min, pressure is maintained at 1.2atm certainly
65 DEG C of pressure releases are so cooled to, sieving can obtain the SiO material coated with ductility carbon material.
Electrochemical property test work is carried out to the anode material of the different matrix of above-described embodiment 1-5 preparation, result is such as
Shown in following table:
| Covering amount (Wt%) | First charge discharge efficiency | Reversible capacity (mAh/g) | 600 weeks circulation conservation rates | |
| SiO(1#) | 3.5% | 77% | 1523 | 93% |
| SnO2-x(2#) | 3.5% | 70% | 1134 | 80% |
| SnO2 | 3.5% | 68% | 715 | 71% |
| Nano-Si-C composite(3#) | 3.5% | 83% | 1136 | 92% |
| Micro Si | 3.5% | 70% | 2683 | 68% |
Claims (11)
1. a kind of preparation method of the Anode of lithium cell material with ductility carbon material cladding, which is characterized in that including following step
It is rapid:
A1, carbon source, the powder core for making anode of lithium ion battery, catalyst are placed in reactor, then are passed through inert gas
Displaced air atmosphere, and by pressure control in 1atm-5atm；
A2, after stable gas pressure and oxygen content is lower than after 200ppm, reactor is warming up in 500-1200 DEG C of temperature range, into
Row catalytic pyrolysis 1-8h；
A3, it is heat-treated in 700-1200 DEG C of temperature range after the completion of catalytic pyrolysis, then by temperature of reactor control
1-8h；
A4,65 DEG C are subsequently cooled to hereinafter, pressure release and go inertia except protective atmosphere, obtain having with what ductility carbon material coated
The lithium ion battery anode material of core-shell structure.
2. a kind of preparation method of Anode of lithium cell material with ductility carbon material cladding according to claim 1,
Be characterized in that: in step A1, the carbon source is one or more small points containing two or more element in C, H, O, N
Sub- organic matter, the small organic molecule contains N element and molecular structure has cyclic structure, including but not limited to heterocyclic compound
Object, pyridines, miazines, the complex compound containing phenyl ring and nitrogen, the object that spreads out of benzene, amide derivatives, heteroaromatic hydrocarbon.
3. a kind of preparation method of Anode of lithium cell material with ductility carbon material cladding according to claim 1,
It is characterized in that: described to be used to that make the powder core of anode of lithium ion battery be in rocking chair type lithium-ion electric pond body in step A1
The active material particle in charge and discharge process with volume expansion, including but not limited to the IVth main group are carried out by removal lithium embedded in system
The simple substance and its derivative of element, the simple substance and its derivative of transition metal element, preferably Si, Sn, C simple substance or its oxidation
Object, and using nano-silicon as function reinforced phase, hard carbon or soft carbon are the micron composite particles of matrix preparation.
4. a kind of preparation method of Anode of lithium cell material with ductility carbon material cladding according to claim 1,
Be characterized in that: in step A1, the carbon source and catalyst are placed in reactor in the form of solid phase or liquid phase, or by carbon source and
Catalyst gasification, and mixed inert gas is passed through in reactor and carries out cracking deposition.
5. a kind of preparation method of Anode of lithium cell material with ductility carbon material cladding according to claim 1,
Be characterized in that: in step A2, it is described heating at the uniform velocity heating or it is non-at the uniform velocity heat up, or in temperature-rise period setting among protect
Warm link, but average heating rate should control 0.2 DEG C per minute to 20 DEG C per minute between.
6. a kind of preparation method of Anode of lithium cell material with ductility carbon material cladding according to claim 1,
Be characterized in that: the inert gas includes nitrogen, argon gas or its mixed gas, and the minute ventilation volume of the inert gas is not
Greater than the 20% of reactor total volume, preferably 0.1%-10%.
7. a kind of preparation method of Anode of lithium cell material with ductility carbon material cladding according to claim 1,
Be characterized in that: the air pressure is constant pressure or pulsed air pressure, and when using pulsed air pressure, the pressure of the air pressure takes intermediate value gas
The pressure difference of pressure, limiting pressure and intermediate value air pressure is not more than ± the 30% of intermediate value air pressure.
8. a kind of preparation method of Anode of lithium cell material with ductility carbon material cladding according to claim 1,
Be characterized in that: the catalyst is one of molybdenum, copper, nickel, iron, cobalt, chromium, platinum, titanium, calcium halophosphate activated by antimony andmanganese, aluminium, silicon simple substance or a variety of lists
Alloy, covalent compound, complex, complex compound or the cyclopentadienyl compounds of matter；The mass fraction of the catalyst is not more than 10%, preferably
For 0.05%-5.5%.
9. a kind of Anode of lithium cell material coated with ductility carbon material, it is characterised in that: the Anode of lithium cell material is
A kind of preparation method of Anode of lithium cell material with ductility carbon material cladding according to claim 1 is prepared
's；The Anode of lithium cell material has core-shell structure；Wherein, shell structure is ductility carbon material clad, the ductility
The class graphite carbon-coating that carbon material clad is adulterated by several layers of N is constituted；Nuclear structure is to pass through in rocking chair type lithium-ion battery system
Removal lithium embedded carries out the active material particle that volume expansion is had in charge and discharge process.
10. a kind of Anode of lithium cell material coated with ductility carbon material according to claim 9, it is characterised in that:
(I) the Anode of lithium cell material has core-shell structure, wherein shell structure is ductility carbon material clad, described to prolong
The class graphite carbon-coating that malleability carbon material clad is adulterated by several layers of N is constituted；
(II) the Anode of lithium cell material has ductility, and the ductility derives from the M type that fold is crimped with multilayer carbon
The ductility carbon material clad that the form of superposition is constituted, the ductility carbon material clad have the multilayer carbon for curling of extending
Nanometer wall array structure；
(III) the Anode of lithium cell material has core-shell structure, wherein nuclear structure is in rocking chair type lithium-ion battery system
The active material particle that volume expansion is had in charge and discharge process is carried out by removal lithium embedded.
11.(IV) outer surface of the Anode of lithium cell material is enclosed with ductility carbon material clad, the ductility carbon materials
The inorganic carbon content of material clad is between 0.5%-10%, the granularity D of the Anode of lithium cell material50It is 4.5-11.5 μm, vibration
Real density is 0.4-1.4 g/cm3, specific surface area is 8-18 m2/g；The reversible capacity 700 of the Anode of lithium cell material ~
68 ~ 92%, 600 weeks 1450mAh/g, first effect circulation conservation rates are greater than 93%.
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| CN113964313A (en) * | 2019-12-30 | 2022-01-21 | 上海杉杉科技有限公司 | Silicon-based negative electrode material and lithium ion battery |
| CN111180693A (en) * | 2019-12-31 | 2020-05-19 | 安普瑞斯（南京）有限公司 | Negative active material, preparation method and application thereof |
| CN111180693B (en) * | 2019-12-31 | 2021-06-04 | 安普瑞斯（南京）有限公司 | Negative active material, preparation method and application thereof |
| WO2023202189A1 (en) * | 2022-04-22 | 2023-10-26 | 贝特瑞新材料集团股份有限公司 | Negative electrode material and preparation method therefor, and lithium-ion battery |
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