CN102867990A - Electrolyte system for preventing spinel lithium titanate radical lithium ion secondary battery from flatulence - Google Patents

Electrolyte system for preventing spinel lithium titanate radical lithium ion secondary battery from flatulence Download PDF

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CN102867990A
CN102867990A CN2011101917828A CN201110191782A CN102867990A CN 102867990 A CN102867990 A CN 102867990A CN 2011101917828 A CN2011101917828 A CN 2011101917828A CN 201110191782 A CN201110191782 A CN 201110191782A CN 102867990 A CN102867990 A CN 102867990A
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lithium
electrolyte system
ion secondary
secondary battery
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索鎏敏
胡勇胜
李泓
陈立泉
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Institute of Physics of CAS
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Abstract

The invention discloses an electrolyte system for preventing a spinel lithium titanate radical lithium ion secondary battery from flatulence. An additive is added into the organic electrolyte system; the additive forms a layer of solid electrolyte interface film on the surface of a Li4Ti5O12 electrode in the battery cyclic process due to the reduction reaction of the organic electrolyte system, so as to prevent a lithium titanate electrode from direct contact with the organic electrolyte, thus the flatulence is prevented; the additive consists of one or more of organic lithium borate salt or boron radical compound as negative iron accepter; and the addition amount of the additive is 0.001-30 wt% of the total electrolyte system. The electrolyte system disclosed by the invention adopts the organic lithium borate salt as the film forming additive of the organic electrolyte, forms a layer of stable SEI (solid electrolyte interface) film on the surface of an active material in the battery cyclic process due to the reduction reaction of the organic electrolyte system, thus the flatulence generation phenomena due to the side reaction of the electrolyte and the active material is prevented, and the cyclic life of the battery is improved.

Description

Prevent the electrolyte system of spinel lithium titanate base lithium ion secondary battery flatulence
Technical field
The invention belongs to the battery technology field.Particularly relate to a kind of for preventing that negative material lithium titanate or modified lithium titanate from producing the electrolyte system of flatulence at circulation and storage process.Has wide application prospect in secondary lithium battery commonly used, power source battery and energy-storage battery field.
Background technology
Lithium ion battery is because the advantage such as its operating voltage is high, energy density is large, have extended cycle life, memory-less effect, pollution-free and self discharge are little, since invention, extremely praise highly, be widely used at present the portable electronics such as mobile phone, notebook computer and video camera.Along with electronics miniaturization and portability, and the appearance of the electric automobile of environmental protection and flourish, lithium ion battery applications market constantly enlarges, future, be accompanied by the develop rapidly of clean energy resource and intelligent grid, lithium ion battery will play a significant role in electric-net valley-electricity and new forms of energy (such as photovoltaic electric, wind-powered electricity generation etc.) storage as a kind of energy storage mode of green economy environmental protection.
What present business-like lithium ion battery negative adopted mainly is as main carbon-based negative electrode material take graphite, because its embedding lithium current potential is very near the sedimentation potential of lithium, operating voltage and the energy density of lithium-ion battery system have been improved to a certain extent, but also just because of this specific character, the deposition of lithium metal can appear in the carbon back negative material on the carbon-based material surface under the high power charging-discharging condition, thereby had a strong impact on its high rate performance, so that there is potential safety hazard in lithium ion battery as electrokinetic cell.Therefore how developing a kind of non-carbon back negative material becomes key.
In numerous non-carbon back negative materials, the Li of spinel-type 4Ti 5O 12Demonstrate unique superiority.Than other negative materials, it has higher lithium ion diffusion coefficient, and lithium ion is deviate from therein and the process that embeds in, volume does not almost change, and is called as a kind of " zero strain material ", good cycling stability.This material electrochemical plateau potential is higher, is about 1.55V (vs Li +/ therefore Li), avoided lithium metal the separating out of negative material surface, its security performance is improved greatly.But also be higher than the current potential that decomposition occurs the organic electrolysis system just because of its discharge voltage, therefore be difficult for forming stable SEI film on the negative material surface.This also just so that this material discharge and recharge and storage process in since between electrode material and the electrolyte because side reaction causes battery flatulence, thereby affect battery life.How to prevent that this material production flatulence from becoming the key of dealing with problems.
Summary of the invention
The object of the present invention is to provide a kind of electrolyte system that prevents spinel lithium titanate base lithium ion secondary battery flatulence.
For achieving the above object, the electrolyte system that prevents spinel lithium titanate base lithium ion secondary battery flatulence provided by the invention, in organic electrolyte system, to add additive, this additive in the circulating battery process since the reduction reaction of organic electrolyte system self at Li 4Ti 5O 12Electrode surface forms one deck solid electrolyte interface film, stops lithium titanate electrode and the direct of organic electrolyte to contact, thus the flatulence of preventing; Additive is the organic boronic lithium salts or forms as one or more of the boryl compound of anion receptor that addition of additive is 0.001～30wt% of electrolyte system total weight.
The described electrolyte system that prevents spinel lithium titanate base lithium ion secondary battery flatulence, wherein, the organic boronic lithium salts is one or more of aryl boric acid lithium, alkylboronic acids lithium.
The described electrolyte system that prevents spinel lithium titanate base lithium ion secondary battery flatulence, wherein, the aryl boric acid lithium comprises: two (catechol) lithium borate (LBBB), two (2,3-is diphenol how) lithium borate (LBNB), two (2,2 '-biphenyl dioxy base) lithium borate (LBBPB), two (salicylic acid) lithium borate (LBSB), two (2,3-pyridine dioxy base) lithium borate (LBPB), perfluor substituted-phenyl three lithium fluoroborate (LiBF 3C 6F 5) in one or more.
The described electrolyte system that prevents spinel lithium titanate base lithium ion secondary battery flatulence, wherein, the alkylboronic acids lithium comprises: one or more in dimalonic acid lithium borate (LiBMB), di-oxalate lithium borate (LiBOB), malonic acid oxalic acid borate (LiMOB), the difluorine oxalic acid boracic acid lithium (LiDFOB).
The described electrolyte system that prevents spinel lithium titanate base lithium ion secondary battery flatulence, wherein, the boryl compound of anion receptor comprises: perfluor replaces one or more in triphenyl borine (TPFPB), the perfluor substituted-phenyl oxalic acid boron (PFPOB).
The described electrolyte system that prevents spinel lithium titanate base lithium ion secondary battery flatulence, wherein, the addition of additive is the 0.1-5wt% of electrolyte system total weight.
The described electrolyte system that prevents spinel lithium titanate base lithium ion secondary battery flatulence, wherein, organic electrolyte system is to be dissolved with lithium salts in organic solvent, employed lithium salts is selected from LiPF 6, LiAsF 6, LiSbF 6, LiBF 4, LiClO 4, LiAlCl 4, LiGaCl 4, LiB 10Cl 10, LiCF 3SO 3, LiC 4F 9SO 3, LiN (C xF 2x+1SO 2) (C yF 2y+1SO 2), LiBF z(CF 3) 4-zOne of, wherein, x and y are natural numbers, z≤4, and the concentration of described lithium salts is 0.5-2.0mol/L.
The described electrolyte system that prevents spinel lithium titanate base lithium ion secondary battery flatulence, wherein, organic solvent in the organic electrolyte system is selected from following organic solvent and composition thereof: propylene carbonate (PC), vinyl carbonate (EC), butylene carbonic ester (BC), methyl ethyl carbonate (EMC), dimethyl carbonate (DMC), diethyl carbonate (DEC), carbonic acid di-n-propyl ester (DPC), carbonic acid diisopropyl ester (DIPC), ethyl propyl carbonic acid ester (EPC), ethylene isopropyl ester (EIPC), oxolane (THF), 2-methyltetrahydrofuran (MeTHF), dimethyl sulfoxide (DMSO) (DMSO), 1, the 3-dioxolanes (1,3-DOL).
The spinel lithium titanate base lithium ion secondary battery system that the electrolyte system that prevents spinel lithium titanate base lithium ion secondary battery flatulence provided by the invention forms can be used on take lithium ion battery as dynamical system and in the energy-storage system.Wherein, dynamical system is: pure electrokinetic cell car and hybrid-power battery car; Energy-storage system is: the energy storage of intelligent grid, clean energy resource wind energy and solar energy.
The present invention is directed to negative material lithium titanate or modified lithium titanate easily produce flatulence in cyclic process problem, proposed to adopt the organic boronic lithium salts as the film for additive of organic electrolyte, so that electrode material and electrolyte react at solid-liquid phase interface, form the stable passivation layer that is covered in electrode material surface of one deck and (be referred to as the solid electrolyte interface film, solid electrolyte interface, be called for short the SEI film), the layer passivating film of formation can stop passing through, deviating from of solvent molecule effectively.Thereby prevent electrolyte and active material because the flatulence phenomenon that causes of side reaction, but Li+ can through this passivation layer freely embed and.Adopt the method will greatly improve negative material and electrolyte in the stability of circulating battery process, the cycle life of battery will be greatly enhanced.
Description of drawings
Fig. 1 is Li of the present invention 4Ti 5O 12The typical first charge-discharge test curve figure of simulated battery system Different adding amount after adopting additive.Wherein V is voltage; MAh/g is capacity.
Fig. 2 is Li of the present invention 4Ti 5O 12The simulated battery system adopts 1M LiPF 6Solvent is EC: DMC=1: added the di-oxalate lithium borate (LiBOB) of 0.1wt% in 1 the electrolyte as the typical recycling life curve figure of additive.Wherein V is voltage; MAh/g is capacity.
Fig. 3 is Li of the present invention 4Ti 5O 12The simulated battery system adopts 1M LiBF 4Solvent is the typical recycling voltammogram that has added 0.2wt% di-oxalate lithium borate (LiBOB) in the electrolyte of PC, sweeps speed and is: 0.05mV/S.
Fig. 4 is Li of the present invention 4Ti 5O 12The simulated battery system has been added the di-oxalate lithium borate (LiBOB) of 0.2wt% as after adding, and head discharges into the typical HRTEM photo behind the 1V week.
Embodiment
Embodiment 1
Li/Li 4Ti 5O 12The system simulated battery, detailed process is as follows:
Respectively take by weighing Li at 8: 1: 1 according to percentage by weight 4Ti 5O 12, acetylene black and Kynoar (PVDF), take pyrrolidones as dispersant, it is mixed.As collector, by roller press mixed slurry is rolled into the pole piece that thickness is 50um with aluminium foil.Electrolyte adopts organic electrolyte EC (ethylene carbonate) and DEC (diethyl carbonate), EC: DEC=1: 1, and electrolyte is 1mol/L LiBF 4, in this system, adding percentage by weight and be 5wt% di-oxalate lithium borate (LiBOB) as film for additive, gained electrolyte water content is lower than 10ppm.
Embodiment 2-6
Respectively take by weighing a certain amount of Li at 8: 1: 1 according to percentage by weight 4Ti 5O 12, acetylene black and Kynoar (PVDF), take pyrrolidones as dispersant, it is mixed.As collector, by roller press mixed slurry is rolled into the pole piece that thickness is 50um with aluminium foil.
Press described in the embodiment 1, the film for additive amount is 0.001wt%, 1wt%, 3wt% and 10wt% respectively, and 30wt%, organic electrolyte solvent are PC (propene carbonate), and electrolyte is 1mol/L LiPF 6, gained electrolyte water content is lower than 10ppm.
Embodiment 7-42
Li/Li 4Ti 5O 12The system simulated battery, detailed process is as follows:
Respectively take by weighing a certain amount of Li at 8: 1: 1 according to percentage by weight 4Ti 5O 12, acetylene black and Kynoar (PVDF), take pyrrolidones as dispersant, it is mixed.As collector, by roller press mixed slurry is rolled into the pole piece that thickness is 50um with aluminium foil.
Press described in the embodiment 1, film for additive adopts two (2 respectively successively, 3-is diphenol how) lithium borate (LBNB), two (2,2 '-biphenyl dioxy base) lithium borate (LBBPB), two (salicylic acid) lithium borate (LBSB), two (2,3-pyridine dioxy base) lithium borate (LBPB), malonic acid oxalic acid borate (LiMOB), two (catechol) lithium borate (LBBB) replaces, addition is followed successively by respectively: 0.001wt%, 1wt%, 3wt% and 10wt%, 30wt%, electrolyte adopts organic electrolyte EC and DMC (dimethyl carbonate), EC: DMC=1: 1, electrolyte is 1mol/L LiBF 4, gained electrolyte water content is lower than 10ppm.
Embodiment 43
Li/Li 4Ti 5O 12The system simulated battery, detailed process is as follows:
Respectively take by weighing a certain amount of Li at 8: 1: 1 according to percentage by weight 4Ti 5O 12, acetylene black and Kynoar (PVDF), take pyrrolidones as dispersant, it is mixed.As collector, by roller press mixed slurry is rolled into the pole piece that thickness is 50um with aluminium foil.Electrolyte adopts organic electrolyte EC and DEC, EC: DEC=1: 1, and electrolyte is 1mol/L LiBF 4, adding percentage by weight in this system is that the 5wt% perfluor replaces triphenyl borine (TPFPB) as film for additive, gained electrolyte water content is lower than 10ppm.
Embodiment 44-47
Respectively take by weighing a certain amount of Li at 8: 1: 1 according to percentage by weight 4Ti 5O 12, acetylene black and Kynoar (PVDF), take pyrrolidones as dispersant, it is mixed.As collector, by roller press mixed slurry is rolled into the pole piece that thickness is 50um with aluminium foil.
Press described in the embodiment 43, the film for additive amount is 0.001wt%, 3wt% and 10wt% respectively, 30wt%, and electrolyte adopts organic electrolyte PC and DMC, PC: DMC=1: 1, electrolyte is 1mol/L LiBF 4, gained electrolyte water content is lower than 10ppm.
Embodiment 48-52
Li/Li 4Ti 5O 12The system simulated battery, detailed process is as follows:
Respectively take by weighing a certain amount of Li at 8: 1: 1 according to percentage by weight 4Ti 5O 12, acetylene black and Kynoar (PVDF), take pyrrolidones as dispersant, it is mixed.As collector, by roller press mixed slurry is rolled into the pole piece that thickness is 50um with aluminium foil.
Press described in the embodiment 43, film for additive adopts perfluor substituted-phenyl oxalic acid boron (PFPOB) to replace, and addition is respectively: 0.001wt%, 1wt%, 3wt% and 10wt%, and 30wt%., electrolyte adopts organic electrolyte PC and DME, PC: DMC=1: 1, and electrolyte is 1mol/L LiCF 3SO 3, gained electrolyte water content is lower than 10ppm.
The comparative example 53
Li/Li 4Ti 5O 12The system simulated battery, detailed process is as follows:
Respectively take by weighing a certain amount of Li at 8: 1: 1 according to percentage by weight 4Ti 5O 12, acetylene black and Kynoar (PVDF), take pyrrolidones as dispersant, it is mixed.As collector, by roller press mixed slurry is rolled into the pole piece that thickness is 50um with aluminium foil.Electrolyte adopts organic electrolyte EC and DMC, EC: DMC=1: 1, and electrolyte is 1mol/L LiPF 6, the electrolyte water content is lower than 10ppm.
Table 1:
Illustration The first week is reversible The first week filled The 2000th week The 2000th week
Embodiment 1 163 92.1 117 84.2
Embodiment 2 165 95.4 136 92.6
Embodiment 3 161 90.4 121 92.8
Embodiment 4 160 89.4 115 85
Embodiment 5 161 87.5 108 79
Embodiment 6 160 87.1 106 75
Embodiment 7 164 93.6 129 94.0
Embodiment 8 160 90.8 121 80.2
Embodiment 9 162 83.8 133 83
Embodiment 159 83.5 115 88.8
Embodiment 154 81.2 106 89.2
Embodiment 153 80 88 78.1
Embodiment 169 91.9 135 94.4
Embodiment 165 90.7 128 92.4
Embodiment 163 82.4 135 93
Embodiment 163 80.2 112 86.6
Embodiment 160 77.2 118 84.5
Embodiment 157 75.1 86 72.9
Embodiment 161 92.1 130 93
Embodiment 162 80 123 94.4
Embodiment 157 87.1 115 84.4
Embodiment 156 87 108 82.8
Embodiment 150 82.8 101 80.9
Embodiment 164 93.6 129 94.0
Embodiment 160 90.8 121 80.2
Embodiment 162 83.8 123 83
Embodiment 159 83.5 115 88.8
Embodiment 155 81.2 106 89.2
Embodiment 153 80 88 78.1
Embodiment 151 73.6 82 72.0
Embodiment 163 92.1 117 84.2
Embodiment 165 95.4 126 92.6
Embodiment 161 90.4 121 92.8
Embodiment 160 89.4 115 85
Embodiment 161 87.5 108 79
Embodiment 160 87.1 106 75
Embodiment 164 93.6 129 94.0
Embodiment 160 90.8 121 80.2
Embodiment 162 83.8 123 83
Embodiment 159 83.5 115 88.8
Embodiment 154 81.2 106 89.2
Embodiment 153 80 88 78.1
Embodiment 169 91.9 135 94.4
Embodiment 165 90.7 128 92.4
Embodiment 163 82.4 125 93
Embodiment 163 80.2 112 86.6
Embodiment 160 77.2 118 84.5
Embodiment 157 75.1 86 72.9
Embodiment 161 92.1 130 93
Embodiment 162 80 123 94.4
Embodiment 157 87.1 115 84.4
Embodiment 155 85.1 109 81.4
Embodiment 165 97.3 Flatulence is serious Flatulence is serious
Annotate: constant current charge is all adopted in above test, the first five week discharges and recharges speed to be: C/5, under 2C, grow circulation subsequently, and since capability retention be to calculate under the 2C and calculated in the 6th week.
Comparative example 53 has used the battery system of additive to compare with other, although the capacity of first all batteries and efficient are slightly high, the flatulence phenomenon is serious in long cyclic process, if without special extrusion process, battery can't obtain 2000 weekly datas.

Claims (10)

1. an electrolyte system that prevents spinel lithium titanate base lithium ion secondary battery flatulence adds additive in organic electrolyte system, this additive in the circulating battery process since the reduction reaction of organic electrolyte system self at Li 4Ti 5O 12Electrode surface forms one deck solid electrolyte interface film, stops lithium titanate electrode and the direct of organic electrolyte to contact, thus the flatulence of preventing;
Additive is the organic boronic lithium salts or forms as one or more of the boryl compound of anion receptor that addition of additive is the 0.001-30wt% of electrolyte system total weight.
2. the described electrolyte system that prevents spinel lithium titanate base lithium ion secondary battery flatulence according to claim 1, wherein, the organic boronic lithium salts is one or more of aryl boric acid lithium, alkylboronic acids lithium.
3. the described electrolyte system that prevents spinel lithium titanate base lithium ion secondary battery flatulence according to claim 2, wherein, the aryl boric acid lithium comprises: two (catechol) lithium borate, two (2,3-is diphenol how) lithium borate, two (2,2 '-biphenyl dioxy base) one or more in lithium borate, two (salicylic acid) lithium borate, two (2,3-pyridine dioxy base) lithium borate, perfluor substituted-phenyl three lithium fluoroborates.
4. the described electrolyte system that prevents spinel lithium titanate base lithium ion secondary battery flatulence according to claim 2, wherein, the alkylboronic acids lithium comprises: one or more in dimalonic acid lithium borate, di-oxalate lithium borate, malonic acid oxalic acid borate, the difluorine oxalic acid boracic acid lithium.
5. the described electrolyte system that prevents spinel lithium titanate base lithium ion secondary battery flatulence according to claim 2, wherein, the boryl compound of anion receptor comprises: perfluor replaces one or more in triphenyl borine, the perfluor substituted-phenyl oxalic acid boron.
6. the described electrolyte system that prevents spinel lithium titanate base lithium ion secondary battery flatulence according to claim 1, wherein, the addition of additive is the 0.1-5wt% of electrolyte system total weight.
7. the described electrolyte system that prevents spinel lithium titanate base lithium ion secondary battery flatulence according to claim 1, wherein, organic electrolyte system is to be dissolved with lithium salts in organic solvent, employed lithium salts is selected from LiPF 6, LiAsF 6, LiSbF 6, LiBF 4, LiClO 4, LiAlCl 4, LiGaCl 4, LiB 10Cl 10, LiCF 3SO 3, LiC 4F 9SO 3, LiN (C xF 2x+1SO 2) (C yF 2y+1SO 2), LiBF z(CF 3) 4-zOne of; Wherein, x and y are natural numbers, z≤4, and the concentration of described lithium salts is 0.5-2.0mol/L.
8. the described electrolyte system that prevents spinel lithium titanate base lithium ion secondary battery flatulence according to claim 7, wherein, organic solvent in the organic electrolyte system is selected from one of following organic solvent or its mixture: propylene carbonate, vinyl carbonate, butylene carbonic ester, methyl ethyl carbonate, dimethyl carbonate, diethyl carbonate, carbonic acid di-n-propyl ester, carbonic acid diisopropyl ester, ethyl propyl carbonic acid ester, ethylene isopropyl ester, oxolane, 2-methyltetrahydrofuran, dimethyl sulfoxide (DMSO), DOX.
9. the spinel lithium titanate base lithium ion secondary battery that forms with the described electrolyte system that prevents spinel lithium titanate base lithium ion secondary battery flatulence of claim 1 is take lithium ion battery as dynamical system with the application in the energy-storage system.
10. application according to claim 9, wherein, dynamical system is: pure electrokinetic cell car and hybrid-power battery car; Energy-storage system is: the energy storage of intelligent grid, clean energy resource wind energy and solar energy.
CN2011101917828A 2011-07-08 2011-07-08 Electrolyte system for preventing spinel lithium titanate radical lithium ion secondary battery from flatulence Pending CN102867990A (en)

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CN102903956A (en) * 2012-10-19 2013-01-30 珠海市赛纬电子材料有限公司 Lithium titanate battery and electrolyte for lithium titanate battery
CN103384018A (en) * 2013-07-19 2013-11-06 四川剑兴锂电池有限公司 Electrolyte capable of reducing gas output of lithium titanate battery
CN103384018B (en) * 2013-07-19 2015-11-04 四川剑兴锂电池有限公司 A kind of electrolyte reducing lithium titanate battery gas production
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CN103840191A (en) * 2014-03-24 2014-06-04 四川兴能新材料有限公司 Lithium titanate battery electrolyte film-forming additive doped with zirconium by gradients
CN108475814A (en) * 2015-09-23 2018-08-31 深圳新宙邦科技股份有限公司 LTO type lithium-ion battery electrolytes
CN106025351A (en) * 2016-07-06 2016-10-12 无锡市宝来电池有限公司 Lithium ion electrolyte safe to use and lithium ion battery
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CN110233289A (en) * 2019-04-04 2019-09-13 李秀艳 A kind of high voltage additive and electrolyte and battery containing the additive
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CN112820940A (en) * 2019-11-15 2021-05-18 华南师范大学 Non-aqueous electrolyte containing 2-fluoro-3-pyridineboronic acid, and lithium metal battery containing same
CN112820940B (en) * 2019-11-15 2022-05-10 华南师范大学 Non-aqueous electrolyte containing 2-fluoro-3-pyridineboronic acid, and lithium metal battery containing same
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CN114229889B (en) * 2021-12-20 2023-11-03 惠州亿纬锂能股份有限公司 Modified titanium-based negative electrode material and preparation method and application thereof

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