CN106972150A - A kind of lithium titanate base lithium ion GND, lithium ion battery and its chemical synthesizing method - Google Patents
A kind of lithium titanate base lithium ion GND, lithium ion battery and its chemical synthesizing method Download PDFInfo
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- H01M10/446—Initial charging measures
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- 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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Abstract
The invention discloses a kind of lithium titanate base lithium ion GND, it is made up of collector and the negative material being coated on the collector, and the negative material is made up of lithium titanate class active material, conductive agent, binding agent and additive；The lithium ion receiving ability of the additive initial charge is more than 2 times of the lithium titanate class active material, and its addition is the 0.2wt% 4wt% of the lithium titanate class active material.The present invention can guarantee that positive electrode capacity gives full play to, so as to improve the design capacity of battery.Additive in the present invention is less than 50% material using first all efficiency for charge-discharges, the lithium ion that it can be absorbed is largely fixed, be not involved in follow-up charge and discharge cycles, so as to which the volume of additive dilation phenomenon repeatedly is mitigated or eliminated, improve thus caused electrode structure destruction, with more preferable cycle life characteristics, accordingly, the present invention also provides a kind of lithium ion battery and its chemical synthesizing method using above-mentioned lithium titanate base lithium ion GND.
Description
Technical field
The invention belongs to field of lithium ion battery, be related to a kind of lithium titanate base lithium ion GND, lithium ion battery and
Its chemical synthesizing method.
Background technology
The promotion of the reasons such as popularization and resource, environmental protection in recent years, with intelligent mobile terminal, lithium ion battery
Obtained a wide range of applications the fields such as electronic product, electric tool, energy storage and electric automobile can be carried.
Lithium titanate as it is a during lithium ion insertion/abjection close to zero strain material, it is super with cycle life
Long advantage；Due to its lithium ion solid-state diffusion speed, thus with cryogenic property, high rate performance is outstanding the characteristics of；Separately
Outside because the current potential of lithium insertion lithium titanate is higher, it is not easy to generate Li dendrite when using as negative pole, so that security compares graphite
Class negative material is high.Therefore, lithium titanate turns into the focus of attention of power energy-storage battery as the battery of negative pole.
From the point of view of the positive pole being engaged with lithium titanate anode, past more use cobalt acid lithium or lithium manganate material, these materials
The characteristics of material is that first all efficiency for charge-discharges are higher, suitable with all efficiency for charge-discharges of the head of lithium titanate anode, therefore using negative pole just
The ratio of pole Capacity Ratio=1.0 will be able to ensure that battery plays maximum capacity and preferably circulation and security feature.
On the other hand, have using nickel, cobalt and manganese oxide lithium salts/nickel cobalt aluminum oxide lithium salts as the tertiary cathode material of representative
The advantages of higher specific capacity, outstanding cycle characteristics and suitable cost performance, have begun to this year and lithium titanate anode phase
Battery is made in matching.As CN104282935A discloses a kind of irregular type ternary material-lithium titanate with high-energy-density
Battery, and advise that the mass ratio of just (negative) pole active material is preferably 1 (for 111 NCM materials, equivalent to negative pole just
Pole Capacity Ratio 1.0；1.0) other ternary material negative pole positive electrode capacity ratios will be less than；CN102074731 discloses a kind of mangaic acid
The battery that lithium and positive pole and the lithium titanate of the mixing of nickel-cobalt-manganese ternary material are constituted, the ratio of wherein ternary material and LiMn2O4 is
30：70.
Because nickel element and elemental lithium easily produce mixing phenomenon in lattice in tertiary cathode material, its first week is caused to be filled
Discharging efficiency is relatively low (90% or so).With first all efficiency for charge-discharge close to 100% lithium titanate anode arrange in pairs or groups when, first week charged
The lithium ion for the irreversible part deviate from journey positive pole can occupy the activity storage lithium site in lithium titanate, therefore, if according to just
The design extremely all made full use of, should use at least 1.10 negative pole positive electrode capacity ratio.This design has used 10% metatitanic acid
Lithium material, and the space that this portion of material is occupied make it that battery design capacity is relatively low；On the other hand, if using 1.00
Negative pole positive electrode capacity ratio, then positive pole be charged to 90% or so negative pole full electric state, i.e. positive pole utilization rate only have 90%, equally
Cause battery design capacity relatively low, and if the overcharge that runaway electric circuit etc. is produced when surprisingly occurring may cause analysis, lithium causes
Security incident.
The content of the invention
It is an object of the invention to for above-mentioned of the prior art not enough negative there is provided a kind of lithium titanate base lithium ion battery
Pole and the lithium ion battery using the lithium titanate base lithium ion GND.
In order to solve the above technical problems, the present invention is adopted the following technical scheme that：
A kind of lithium titanate base lithium ion GND, it is by collector and the negative material structure being coated on the collector
Into the negative material is made up of lithium titanate class active material, conductive agent, binding agent and additive；The additive fills first
The lithium ion receiving ability of electricity is more than 2 times of the lithium titanate class active material, and its addition is lithium titanate class activity
The 0.2wt%-4wt% of material.
Further, the additive all efficiency for charge-discharges first to lithium ion are less than 50%.
Further, the additive is in carbon material, silicon, Si oxide, tin, tin-oxide, transition metal oxide
One or several kinds.
Further, described carbon material uses hard carbon, soft carbon, graphite, the one or more of graphene.
Further, described Si oxide is the one or more in the sub- silicon of oxidation, polyoxy SiClx.
Further, described tin-oxide is the one or more in stannous oxide, tin ash.
Further, described transition metal oxide is oxide, the oxide of cobalt, the oxide of nickel, the tungsten of iron
One or more in oxide, titanyl compound, the oxide of vanadium, the oxide of manganese, the oxide of copper.
A kind of lithium ion battery, it is using the lithium titanate base lithium ion GND as described in above-mentioned scheme.
A kind of chemical synthesizing method of lithium ion battery using above-mentioned lithium titanate base lithium ion GND：At least once
Charging voltage V meets Vmax-1.3 volts<V≤Vmax, the Vmax allow charging for the highest of positive electrode opposing metallic lithium
Voltage.
The beneficial effects of the present invention are：
1st, when the lithium titanate base lithium ion GND and low first all efficiency positive pole composition batteries of the class of ternary material one
When, in formation process during first week charging, the additive can receive more to be moved by positive pole than lithium titanate class active material
The lithium ion of in-migration, so that even excessively than under the conditions of also can guarantee that positive electrode capacity gives full play in less negative pole, so that
Improve the design capacity of battery.
2nd, the addition of described additive is the 0.2wt%-4wt% of the lithium titanate class active material；If addition
Amount very little, due to its absorb positive pole migration come lithium ion ratio very little so that improve positive electrode capacity performance effect it is little；
If addition is too big, because additive also takes up space in itself, it will make it that the effect for improving battery design capacity is little very
The design capacity of battery may extremely be reduced.
3rd, because the additive may be also the active material that inserts/deviate from ability with lithium ion in itself, if
Lithium ion in the charge and discharge process additive of battery also assists in insertion/abjection, it would be possible to the discrepancy of the lithium ion addition
The volume of agent dilation repeatedly, so as to cause electrode structure to be destroyed.Therefore the additive is imitated using first all discharge and recharges
Rate is less than 50% material, and the lithium ion that can be absorbed it is largely fixed, be not involved in follow-up charge and discharge cycles, so that
The volume of additive dilation phenomenon repeatedly is mitigated or eliminated, improves thus caused electrode structure destruction, with more
Good cycle life characteristics.
4th, because lithium titanate anode current potential 1.55V higher than lithium metal or so, the maximum charging voltage being generally melted into is positive pole
To the highest charging Vmax-1.55V of lithium metal.For the additive, lithium ion may be still not enough under this voltage conditions
To insert, therefore voltage U meets Vmax-1.3 volts to formation process at least once<V≤Vmax, can cause lithium ion to insert
And be fixed in the additive, so as to play good effect.
Embodiment
The invention discloses a kind of lithium titanate base lithium ion GND, it is by collector and is coated on the collector
Negative material is constituted, and the negative material is made up of lithium titanate class active material, conductive agent, binding agent and additive；It is described to add
Plus more than 2 times that the lithium ion receiving ability of agent initial charge is the lithium titanate class active material, its addition is the titanium
The 0.2wt%-4wt% of sour lithium class active material.
Preferably the additive all efficiency for charge-discharges first to lithium ion are less than 50%.
Preferably, the additive is carbon material, silicon, Si oxide, tin, tin-oxide, transiting metal oxidation
One or several kinds in thing.
Preferably, described carbon material uses hard carbon, soft carbon, graphite, the one or more of graphene.
Preferably, described Si oxide is the one or more in the sub- silicon of oxidation, polyoxy SiClx.
Preferably, described tin-oxide is the one or more in stannous oxide, tin ash.
Preferably, described transition metal oxide be the oxide of iron, the oxide of cobalt, the oxide of nickel,
One or more in the oxide of tungsten, titanyl compound, the oxide of vanadium, the oxide of manganese, the oxide of copper.
A kind of lithium ion battery, it is using such as the lithium titanate base lithium ion GND in above-mentioned scheme.
A kind of chemical synthesizing method of lithium ion battery using above-mentioned lithium titanate base lithium ion GND：At least once
Charging voltage V meets Vmax-1.3 volts<V≤Vmax, the Vmax allow charging for the highest of positive electrode opposing metallic lithium
Voltage.
The present invention is described in detail with reference to specific embodiment and comparative example (by taking making of 18650 lithium ion batteries as an example)
Content.
(addition of additive described in the present embodiment is about the lithium titanate class active material to embodiment 1
0.2wt%)
Negative electrode of lithium ion battery makes：
13.5gPVDF is added in 550mL NMP, dissolving is sufficiently stirred for；4.5g conductive blacks are added to stir 30 minutes；Plus
Enter 449.1g lithium titanate materials (capacity 165mAh/g), (half-cell surveys initial charge capacity to the sub- Si powder of the commercially available oxidations of 0.9g
2380mAh/g, first week efficiency 33.7%), stir 60 minutes.Above the aluminium foil that obtained slurry is coated on to 20 microns of thickness,
120 degree of oven for drying, coating weightening is 220g/m2 (two sides).
It is compacted by density 2.0, is cut into 57mm width.
The making of lithium ion battery：
12g PVDF are added in 350mL NMP, dissolving is sufficiently stirred for；12g conductive blacks are added to stir 30 minutes；Add
(capacity 165mAh/g, first week efficiency 89%, opposing metallic lithium highest allows charging electricity to the commercially available NMC622 tertiary cathode materials of 800g
Press Vmax=4.25V), stir 100 minutes.
Above the aluminium foil that obtained slurry is coated on to 20 microns of thickness, negative pole titanium is pressed in 120 degree of oven for drying, coating weightening
Sour lithium material correspondence capacity：Positive pole ternary material correspondence capacity=1.00 are calculated.
It is compacted by compacted density 3.5, is cut into width 56mm.
Barrier film uses 16 micron thickness, 60mm width, the PE micro-pore septums of porosity 45%.
Positive pole, negative pole are wound between barrier film, internal diameter 17.4mm, external diameter 18.0mm, height 65.0 is then charged into
In box hat, the length of both positive and negative polarity is cut by the assembling elasticity to box hat internal diameter 92%.
Inject 5g 1mol/L LiPF6 electrolyte (solvent EC：EMC：DEC=1：1：1).
The block of 18650 lithium ion batteries is loaded onto, sealing is then carried out closed.
Shelve after 2 hours, charged with 300mA, 4.20V (30mA cut-offs) CCCV, 300mA, 1.60V constant-current discharge
Into obtained 18650 lithium ion batteries.
Embodiment 2 (addition of additive described in the present embodiment is about the 1wt% of the lithium titanate class active material)
The making of lithium titanate base lithium ion GND：
13.5gPVDF is added in 550mL NMP, dissolving is sufficiently stirred for；4.5g conductive blacks are added to stir 30 minutes；Plus
Enter 445.5g lithium titanate materials (capacity 165mAh/g), the commercially available tin ash of 4.5g (half-cell actual measurement head fills capacity 1350mAh,
First week efficiency 31%) powder, is stirred 60 minutes.Above the aluminium foil that obtained slurry is coated on to 20 micron thickness, 120 degree of baking ovens
Drying, coating weightening is 220g/m2 (two sides).
It is compacted by density 2.0, is cut into 57mm width
The making of 18650 lithium ion batteries：
Step be the same as Example 1.
Embodiment 3 (addition of additive described in the present embodiment is about the 2wt% of the lithium titanate class active material)
13.5gPVDF is added in 550mL NMP, dissolving is sufficiently stirred for；4.5g conductive blacks are added to stir 30 minutes；Plus
Enter 441g lithium titanate materials (capacity 165mAh/g), the commercially available nickel protoxide powder of 9g (actual measurement initial charge capacity 980mAh/g, head
All efficiency 38.1%), stir 60 minutes.Above the aluminium foil that obtained slurry is coated on to 20 micron thickness, 120 degree of baking ovens dry
Dry, coating weightening is 220g/m2 (two sides).
It is compacted by density 2.0, is cut into 57mm width.
The making of 18650 lithium ion batteries：
Step be the same as Example 1.
Embodiment 4 (addition of additive described in the present embodiment is about the 4wt% of the lithium titanate class active material)
13.5gPVDF is added in 550mL NMP, dissolving is sufficiently stirred for；4.5g conductive blacks are added to stir 30 minutes；Plus
Enter 432g lithium titanate materials (capacity 165mAh/g), the commercially available hard carbon powder of 18g (actual measurement initial charge capacity 430mAh/g, first week
Efficiency 73.1%), stir 60 minutes.Above the aluminium foil that obtained slurry is coated on to 20 micron thickness, 120 degree of oven for drying,
Coating weightening is 220g/m2 (two sides).
It is compacted by density 2.0, is cut into 57mm width.
The making of 18650 lithium ion batteries：
In addition to chemical conversion, step be the same as Example 1.
Chemical synthesis technology is：Shelve after 2 hours, charged with 300mA, 3.0V (30mA cut-offs) CCCV, 300mA, 1.60V constant current
Electric discharge is melted into, and 18650 lithium ion batteries are made.
Comparative example 1：
Negative electrode of lithium ion battery makes：
13.5gPVDF is added in 550mL NMP, dissolving is sufficiently stirred for；4.5g conductive blacks are added to stir 30 minutes；Plus
Enter 450g lithium titanate materials (capacity 165mAh/g), stir 60 minutes.Obtained slurry is coated on to the aluminium foil of 20 micron thickness
Above, 120 degree of oven for drying, coating weightening is 220g/m2 (two sides).
It is compacted by density 2.0, is cut into 57mm width.
The making of lithium ion battery：
12g PVDF are added in 350mL NMP, dissolving is sufficiently stirred for；12g conductive blacks are added to stir 30 minutes；Add
(capacity 165mAh/g, first week efficiency 89%, opposing metallic lithium highest allows charging electricity to the commercially available NMC622 tertiary cathode materials of 800g
Press Vmax=4.25V), stir 100 minutes.
Above the aluminium foil that obtained slurry is coated on to 20 microns of thickness, negative pole titanium is pressed in 120 degree of oven for drying, coating weightening
Sour lithium material correspondence capacity：Positive pole ternary material correspondence capacity=1.00 are calculated.
It is compacted by compacted density 3.5, is cut into width 56mm.
Barrier film uses 16 micron thickness, 60mm width, the PE micro-pore septums of porosity 45%.
Positive pole, negative pole are wound between barrier film, internal diameter 17.4mm, external diameter 18.0mm, height 65.0 is then charged into
In box hat, the length of both positive and negative polarity is cut by the assembling elasticity to box hat internal diameter 92%.
Inject 5g 1mol/L LiPF6 electrolyte (solvent EC：EMC：DEC=1：1：1).
The block of 18650 lithium ion batteries is loaded onto, sealing is then carried out closed.
Shelve after 2 hours, charged with 300mA, 2.80V (30mA cut-offs) CCCV, 300mA, 1.60V constant-current discharge
Into the battery of comparative example 1 of obtained 18650 models.
Comparative example 2：
Negative electrode of lithium ion battery makes：
With comparative example 1.
18650 lithium ion batteries make：
12g PVDF are added in 350mL NMP, dissolving is sufficiently stirred for；12g conductive blacks are added to stir 30 minutes；Add
The commercially available NMC622 tertiary cathode materials of 800g (capacity 165mAh/g, first week efficiency 89%), are stirred 100 minutes.
Above the aluminium foil that obtained slurry is coated on to 20 micron thickness, negative pole stone is pressed in 120 degree of oven for drying, coating weightening
Ink material correspondence capacity：Positive pole ternary material correspondence capacity=1.10 are calculated.It is cut into 56mm width.
Barrier film uses 16 micron thickness, 60mm width, the PE micro-pore septums of porosity 45%.
Positive pole, negative pole are wound between barrier film, internal diameter 17.4mm, external diameter 18.0mm, height 65.0 is then charged into
In box hat, the length of both positive and negative polarity is cut by the assembling elasticity to box hat internal diameter 92%.
Inject 5g 1mol/L LiPF6 electrolyte (solvent EC：EMC：DEC=1：1：1).
The block of 18650 lithium ion batteries is loaded onto, sealing is then carried out closed.
Shelve after 2 hours, charged with 300mA, 2.80V (30mA cut-offs) CCCV, 300mA, 1.60V constant-current discharge
Into the obtained battery of comparative example 2.
Embodiment 1-3 and comparative example 1-2 battery are discharged into after 1.6V with 300mA, with 60 points of 4500mA constant-current charges
Clock (max10V) carries out overcharge test, and whether observation battery occurs combustion explosion event.
Another power taking pond is charged with 7.5A 2.8V (30mA cut-offs) CCCV at ambient temperature, 7.5A 1.6V constant-current discharges,
Circulation 500 weeks, calculates battery capacity conservation rate.
As a result it is as shown in the table：
Obtained 18650 lithium ion batteries are keeping cycle life and mistake in embodiment 1-4 it can be seen from the above
It can be obtained than the higher capacity of comparative example 1 and 2 on the premise of charging safety；In addition, if lithium titanate anode matches somebody with somebody tertiary cathode
Using 1.00 negative pole positive electrode capacity ratio (comparative example 1), then exploded in overcharge test.
In summary, the present invention can effectively improve positive pole (such as ternary material that lithium titanate anode coordinates low first all efficiency
Positive pole) high-capacity battery is made, while keep its cycle characteristics and security feature not to deteriorate, therefore with obvious economic valency
Value.
The present invention is easy to implement, it is with low cost, be easy to industrialized production.
The above description of this invention and application be illustrative, be not wishing to limit the scope of the invention to above-mentioned implementation
In example.In the case where not departing from scope and spirit of the present invention, can to embodiments disclosed herein carry out it is other deformation and
Change.
Claims (9)
1. a kind of lithium titanate base lithium ion GND, it is made up of collector and the negative material being coated on the collector,
The negative material is made up of lithium titanate class active material, conductive agent, binding agent and additive；It is characterized in that：The addition
The lithium ion receiving ability of agent initial charge is more than 2 times of the lithium titanate class active material, and its addition is the metatitanic acid
The 0.2wt%-4wt% of lithium class active material.
2. lithium titanate base lithium ion GND according to claim 1, it is characterised in that：The additive is to lithium ion
First week efficiency for charge-discharge is less than 50%.
3. lithium titanate base lithium ion GND according to claim 1 or 2, it is characterised in that：The additive is carbon
One or several kinds in material, silicon, Si oxide, tin, tin-oxide, transition metal oxide.
4. lithium titanate base lithium ion GND according to claim 3, it is characterised in that：Described carbon material is using hard
Carbon, soft carbon, graphite, the one or more of graphene.
5. lithium titanate base lithium ion GND according to claim 3, it is characterised in that：Described Si oxide is oxygen
Change the one or more in sub- silicon, polyoxy SiClx.
6. lithium titanate base lithium ion GND according to claim 3, it is characterised in that：Described tin-oxide is oxygen
Change the one or more in stannous, tin ash.
7. lithium titanate base lithium ion GND according to claim 3, it is characterised in that：Described transiting metal oxidation
Thing is oxide, the oxide of cobalt, the oxide of nickel, the oxide of tungsten, titanyl compound, the oxide of vanadium, the oxygen of manganese of iron
One or more in compound, the oxide of copper.
8. a kind of lithium ion battery, it is characterised in that：It is using the lithium titanate base lithium as any one of claim 1 to 7
Ion battery negative pole.
9. a kind of lithium ion battery of lithium titanate base lithium ion GND using as any one of claim 1 to 7
Chemical synthesizing method, it is characterised in that：Charging voltage V meets Vmax-1.3 volts at least once<V≤Vmax, the Vmax are
The highest of positive electrode opposing metallic lithium allows charging voltage.
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| CN107910489A (en) * | 2017-11-28 | 2018-04-13 | 广东省肇庆市质量计量监督检测所 | A kind of lithium ion battery negative material and preparation method thereof |
| CN110911732A (en) * | 2018-09-16 | 2020-03-24 | 深圳格林德能源有限公司 | Long-life high-capacity silicon negative electrode lithium ion battery |
| CN111313004A (en) * | 2020-02-28 | 2020-06-19 | 陕西煤业化工技术研究院有限责任公司 | Silicon monoxide-lithium titanate-based composite negative electrode material for lithium ion battery and preparation method thereof |
| CN112768628A (en) * | 2021-02-05 | 2021-05-07 | 远景动力技术(江苏)有限公司 | Positive pole piece and preparation method and application thereof |
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| CN104577044A (en) * | 2014-11-18 | 2015-04-29 | 深圳市金润能源材料有限公司 | Lithium titanate battery and preparation method thereof |
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