CN102867983A - Nonaqueous secondary lithium battery - Google Patents
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- CN102867983A CN102867983A CN2011101848512A CN201110184851A CN102867983A CN 102867983 A CN102867983 A CN 102867983A CN 2011101848512 A CN2011101848512 A CN 2011101848512A CN 201110184851 A CN201110184851 A CN 201110184851A CN 102867983 A CN102867983 A CN 102867983A
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a nonaqueous secondary lithium battery, its anode active material is a composite material of a carbon material and crystal form or amorphous form ferric phosphate, its cathode active material is a silicon lithium alloy capable of existing in a stable mode in air, or a composite of carbon and lithium metal, or a lithium metal membrane deposited on a copper current collector, or lithium metal adhered on the foam copper current collector. The nonaqueous secondary lithium battery has the advantages of safety, low cost, high power, high energy density and stable circularity, and has good application prospect.
Description
Technical field
The present invention relates to a kind of nonaqueous secondary lithium battery, the composite material of this Battery carbon material and crystalline form or unformed ferric phosphate is done anodal, and positive pole does not contain lithium, does negative pole with lithium-containing materials, has high-energy-density, the advantage such as high magnification characteristic and long cycle performance and preparation cost are cheap.
Prior art
Making anodal lithium ion battery with LiFePO 4 develops rapidly in recent years.Ferrousphosphate lithium material is made lithium battery anode and is reported in the people's such as Goodenough patent US-5910382.Pure crystal formation ferrousphosphate lithium material be almost do not have electroactive, only have the LiFePO 4 nanometer, and coated with conductive carbon-coating or the LiFePO 4 particle is attached to just can makes it obtain higher specific capacity on the conduction Carbon Materials of high-ratio surface, such as the people such as Guo Yuguo report (Adv.Mater.2009,21,2710) charcoal-lithium ferrous phosphate composite material discharges under the high magnification of 230C and still can emit the specific capacity of 60mAh/g.The ferrousphosphate lithium material discharge voltage is lower, and cyclical stability is good, and fail safe is good, is one of first-selected positive electrode of electrokinetic cell.Yet the method for charcoal-lithium iron phosphate composite electrode material is covered at the patent CN100421289C of China's application by Quebec, CAN water power company at present.In addition, ferro element is in reduction-state in the LiFePO 4, and is unstable in air, cause this material require comparatively preparing, keeping under the exacting terms, and the repeatability of material industry production is not good, causes cost not low.
Different from the LiFePO 4 situation, iron is in the trivalent oxidation state in the ferric phosphate, and existence that can be stable in air, and preparation technology is simple is with low cost, has become the important source material of synthesizing lithium ferrous phosphate.In recent years, researcher's work shows, crystal formation or the ferric phosphate of unformed people such as (, Materials Research Bulletin 2002,37,1249) Whittingham can both embody excellent chemical property.Kang (Adv.Mater.2010,22,5537) etc. the iron phosphate nano particle is attached on the tubulose Carbon Materials, ferric phosphate obtains the above specific discharge capacity of 150mAh/g and excellent cyclical stability, performance and ferrousphosphate lithium material are suitable, but have no the report of making lithium battery.
It is the method that raw material prepares ferric phosphate with metallic iron that the people such as the heavy people in field, ridge have reported a kind of at Chinese patent CN1706056, and this patent application does not relate to the content of charcoal coating and energy storage system construction aspect.
The poorly conductive of ferric phosphate can significantly improve its chemism and cyclical stability with its nanometer and carbon coated conductive layer.Do positive active material with charcoal-ferric phosphate composite material, the good negative material of collocation performance can obtain high performance serondary lithium battery, and good industrial prospect is arranged.Yet different from LiFePO 4, ferric phosphate positive pole does not contain lithium ion, needs negative material to contain lithium ion or comprises lithium metal, namely contains cathode of lithium.
Containing aspect the cathode of lithium research Huggins (Solid State Ionics 1998,113-115,57) reported for work preparation and the performance of silicon lithium alloy negative pole.Lithium content is higher than 40% in this silicon lithium alloy, but it is very unstable in air, and the difficulty that processing stores and cost increase.The paper of Huggins is not mentioned the problem of lithium battery system collocation.The people such as Yang Jun are at the paper of delivering recently (Acta PhySico-Chimica Sinica, 2011,27,759) method with electro-deposition in has prepared silicon-cathode of lithium material, studies show that this material has advantages of height ratio capacity and good circulation stability, but do not mention the problem of positive electrode collocation aspect.Announce the preparation method of a series of metals-lithium alloy negative pole in the US Patent No. 4326335, but do not comprised silicon-lithium alloy negative pole.
Lithium metal and charcoal is compound, can provide a large amount of lithium ions for the SEI film forms, thereby improve the specific energy of lithium battery.(the Electrochimica Acta 2007 such as He Xiangming, 52,4312) reported the charcoal-application of lithium combination electrode in lithium ion battery, but the making of this electrode is the surface that simply the lithium paper tinsel is pressed together on the charcoal negative plate, may produce a large amount of heat when carbon and two kinds of active material pressings of lithium and potential safety hazard is arranged.
At present lithium battery is all done negative pole with metallic lithium foil, and this type of electrode specific surface is little, and high rate performance is relatively poor, and easily produces dendrite and cause potential safety hazard.Lithium metal evenly is attached in the foam copper with graininess, can effectively increases the reaction interface of lithium, and be difficult for producing dendrite, and then obtain high magnification and preferably fail safe.
The specific capacity 160mAh/g of ferric phosphate is far below the specific capacity of lithium metal.If make positive pole with charcoal-ferric phosphate composite material, the lithium metal film is done negative pole and is made lithium battery, and the thickness of negative pole lithium metal film is attenuate significantly.The lithium paper tinsel negative pole thickness that general lithium battery is used surpasses 100 μ m more, and this has caused the waste of active material on the one hand, and thicker pole piece occupies the larger volume of battery on the other hand.Method with physical deposition can obtain the lithium sedimentary deposit that thickness is lower than 100 μ m, has not only effectively reduced the unnecessary waste of active material, can also make lithium battery obtain better high rate performance.
The Carbon Materials such as carbonaceous mesophase spherules, graphite, hard charcoal are lithium ion battery negative materials commonly used, but specific capacity is lower, and can form the SEI film and expend a large amount of lithium ions in the charcoal negative terminal surface in the embedding lithium process first.Be the composite negative pole of the thin slice of base material and barrier film and the combination of lithium metal thin slice by charcoals such as hard charcoals, lithium can provide a large amount of lithium ions for the SEI film forms, and avoids the capacitance loss behind the first charge-discharge; Charcoal can provide high embedding-Tuo lithium surface area, improves the battery multiplying power property, avoids the generation of Li dendrite; Barrier film intercepts carbon plate and contacts with the direct of metal lithium sheet, improves fail safe.
Summary of the invention
The purpose of this invention is to provide a kind of high rate capability, high-energy-density, the serondary lithium battery of the non-aqueous system of good cycle performance and preferably fail safe.
A kind of nonaqueous secondary lithium battery provided by the invention comprises this battery and comprises positive pole, negative pole and barrier film, positive pole is comprised of anode electrode sheet and collector, the anode electrode sheet is comprised of positive active material, conductive agent and binding agent, positive active material is the composite material of charcoal and ferric phosphate, ferric phosphate is crystalline form or unformed, exists with the form of particle, and particle is 0.01～20 μ m, charcoal is carbon nano-tube, carbon black, active carbon or the Graphene of hole prosperity, and the porosity of charcoal is 0.5～5.0cm
3/ g, iron phosphate grains are attached in the hole of charcoal and outer surface, and perhaps charcoal is coated on the iron phosphate grains outer surface with the thickness of 0.002～0.1 μ m; Negative pole is comprised of negative electricity pole piece and collector, the negative electricity pole piece is comprised of negative electrode active material, conductive agent and binding agent, and negative electrode active material is the composite material of silicon lithium alloy, charcoal and lithium metal, at lithium metal film that copper current collector deposits or be attached to lithium metal on the foam copper collector.
The negative electrode active material silicon lithium alloy of nonaqueous secondary lithium battery of the present invention exists with the form of 0.01～10 μ m particulate, and the lithium percentage by weight is 5～45% in the silicon lithium alloy.
Charcoal is porous charcoal, MCMB or graphite in the negative electrode active material charcoal of nonaqueous secondary lithium battery of the present invention and the lithium metal composite material, and the porous charcoal porosity is 0.5～5.0cm
3/ g, lithium metal are attached in the endoporus of porous charcoal and outer surface, and the lithium metal percentage by weight is 8～55%; Carbonaceous mesophase spherules or graphite exist with the electrode slice form, and thickness is 5～300 μ m, and one deck barrier film is covered on its surface, enclose the lithium metal thin slice on the barrier film again and form negative pole, and the lithium metal sheet thickness is 0.1～200 μ m.
The lithium metal film thickness that the negative electrode active material of nonaqueous secondary lithium battery of the present invention deposits at copper current collector is 0.1～200 μ m; The hole count (PPI) of negative electrode active material foam copper collector per inch is 10～400, and thickness is 0.02～2.0mm, and lithium metal exists with the form of particle, and particle is of a size of 0.1～100 μ m.
Conductive agent of the present invention is graphite or acetylene black, and binding agent is Kynoar or polytetrafluoroethylene.
Nonaqueous secondary lithium battery of the present invention has safety, low cost, high power, the advantage of high-energy-density and stable cycle performance.The battery specific energy reaches more than the 80Wh/kg, and capability retention is more than 60% under 5C, circulates 100 capacity attenuations below 15%, and good application prospect is arranged.
Description of drawings
Fig. 1 is planar structure schematic diagram of the present invention
1. plus plate current-collecting body, 2. negative current collector, 3. anode electrode sheet, 4. negative electricity pole piece, 5. barrier film
Fig. 2 is the ESEM picture of charcoal and ferric phosphate anode composite among the present invention
Fig. 3 is that charcoal coats the unformed and charging and discharging curve of crystal formation ferric phosphate positive pole material in ethyl carbonate (EC) solution of LiBF4 among the present invention
Abscissa: discharge capacity; Ordinate: electrode potential (take lithium metal as reference electrode).
Embodiment
Lithium battery positive pole active substance is that charcoal coats the ferric phosphate material, and ferric phosphate is unformed shape, is graininess, and size 0.2～2 μ m, charcoal coating thickness are 0.005 μ m.Negative electrode active material is silicon lithium alloy particulate, and particle size is 10 μ m, and lithium content is 21% (weight ratio) in the alloy.The positive and negative electrode conductive agent is acetylene black, and binding agent is Kynoar.All with the coating method preparation, the thickness of both positive and negative polarity electrode slice is 100 μ m to the battery positive and negative electrode, and electrolyte is LiBF
4Ethyl carbonate (EC) solution, concentration is 1mol/L.The operating voltage interval of 18650 type batteries is 2.5～3.6V, and the battery specific energy is 105Wh/kg, and capability retention is 75% under 5C, and capacity attenuation 7% circulates 100 times.
Embodiment 2
Lithium battery positive pole active substance is carbon nano-tube-ferric phosphate composite material, and carbon nano-tube is standby with the floating catalytic legal system, average length 25 μ m, and ferric phosphate is crystal formation, is graininess, size 8 μ m are attached on the carbon nano-tube to the ferric phosphate uniform crystal particles.Negative active core-shell material is charcoal and lithium metal composite material, and Carbon Materials is the active carbon of the hole prosperity of template synthesis, and porosity is 2.3cm
3/ g, the lithium metal uniform particles is attached in the endoporus of Carbon Materials and outer surface, and average-size is 2 μ m, and lithium content is 25% weight ratio in the composite material.The positive and negative electrode conductive agent is graphite, and binding agent is Kynoar.All with the coating method preparation, the thickness of both positive and negative polarity electrode slice is 120 μ m to the battery positive and negative electrode, and electrolyte is LiBF
4Diethyl carbonate (DEC) solution, concentration is 1.2mol/L.The operating voltage interval of flexible-packed battery is 2.4～3.5V, and the battery specific energy is 93Wh/kg, and capability retention is 82% under 5C, and capacity attenuation 6% circulates 100 times.
Embodiment 3
Lithium battery positive pole active substance is Graphene-ferric phosphate composite material, and Graphene is standby with the electric arc legal system, and the lamella average-size is 0.2 μ m, and ferric phosphate is crystal formation, is graininess, size 0.1 μ m, being attached on the Graphene of ferric phosphate uniform crystal particles.Anode prepares with coating method, and the thickness of anode electrode sheet is 60 μ m.Anodal conductive agent is acetylene black, and binding agent is Kynoar.Negative active core-shell material is the lithium metal film that deposits at copper current collector, and the thickness of lithium film is 12 μ m.Electrolyte is LiBF
4Ethyl carbonate (EC) and diethyl carbonate (DEC) solution (EC and DEC volume ratio are 1: 1), concentration is 1.5mol/L.The operating voltage interval of flexible-packed battery is 2.6～3.6V, and the battery specific energy is 80Wh/kg, and capability retention is 90% under 5C, and capacity attenuation 10% circulates 100 times.
Embodiment 4
Lithium battery positive pole active substance is charcoal-ferric phosphate composite material, and Carbon Materials is the active carbon that graininess is rich in macropore, and particle mean size is 50 μ m, ferric phosphate is unformed shape, be graininess, size 1 μ m, the ferric phosphate uniform crystal particles be attached to active carbon outer surface and inner large internal surface of hole.Anode prepares with coating method, and anode electrode sheet thickness is 100 μ m.Anodal conductive agent is acetylene black, and binding agent is Kynoar.Negative electrode active material is the lithium metal particulate that is attached on the foam copper collector, lithium metal exists with the form of particle, and particle is of a size of 10 μ m, and foam copper collector pore size distribution density is 200 of per inch, hole dimension is 50 μ m, and foam copper collector thickness is 1.0mm.Electrolyte is LiPF
6Ethyl carbonate (EC) and dimethyl carbonate (DMC) solution (EC and DMC volume ratio are 1: 1), concentration is 1.0mol/L.The operating voltage interval of flexible-packed battery is 2.6～3.7V, and the battery specific energy is 110Wh/kg, and capability retention is 88% under 5C, and capacity attenuation 9% circulates 100 times.
Claims (6)
1. nonaqueous secondary lithium battery, it is characterized in that this battery comprises positive pole, negative pole and barrier film (5), positive pole is comprised of anode electrode sheet (3) and collector (1), the anode electrode sheet is comprised of positive active material, conductive agent and binding agent, positive active material is the composite material of charcoal and ferric phosphate, ferric phosphate is crystalline form or unformed, form with particle exists, particle is 0.01～20 μ m, charcoal is carbon nano-tube, carbon black, active carbon or the Graphene of hole prosperity, and the porosity of charcoal is 0.5～5.0cm
3/ g, iron phosphate grains are attached in the hole of charcoal and outer surface, and perhaps charcoal is coated on the iron phosphate grains outer surface with the thickness of 0.002～0.1 μ m; Negative pole is comprised of negative electricity pole piece (4) and collector (2), the negative electricity pole piece is comprised of negative electrode active material, conductive agent and binding agent, and negative electrode active material is the composite material of silicon lithium alloy, charcoal and lithium metal, at lithium metal film that copper current collector deposits or be attached to lithium metal on the foam copper collector.
2. nonaqueous secondary lithium battery according to claim 1 is characterized in that the silicon lithium alloy exists with the form of 0.01～10 μ m particulate, and the lithium percentage by weight is 5～45% in the silicon lithium alloy.
3. nonaqueous secondary lithium battery according to claim 1 is characterized in that charcoal is porous charcoal, MCMB or graphite in the composite material of negative electrode active material charcoal and lithium metal, and the porous charcoal porosity is 0.5～5.0cm
3/ g, lithium metal are attached in the endoporus of porous charcoal and outer surface, and the lithium metal percentage by weight is 8～55%; Carbonaceous mesophase spherules or graphite exist with the electrode slice form, and thickness is 5～300 μ m, and one deck barrier film (5) is covered on its surface, enclose the lithium metal thin slice on the barrier film (5) again and form negative pole, and the lithium metal sheet thickness is 0.1～200 μ m.
4. nonaqueous secondary lithium battery according to claim 1 is characterized in that the lithium metal film thickness that deposits at copper current collector is 0.1～200 μ m.
5. nonaqueous secondary lithium battery according to claim 1 is characterized in that the hole count (PPI) of foam copper collector per inch is 10～400, and thickness is 0.02～2.0mm, and lithium metal exists with the form of particle, and particle is of a size of 0.1～100 μ m.
6. nonaqueous secondary lithium battery according to claim 1, the conductive agent that it is characterized in that this battery is graphite or acetylene black, binding agent is Kynoar or polytetrafluoroethylene.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104937756A (en) * | 2013-01-23 | 2015-09-23 | 东丽株式会社 | Positive electrode active material/graphene composite particles, and positive electrode material for lithium ion battery |
| CN107221709A (en) * | 2017-06-09 | 2017-09-29 | 清华大学 | The lithium metal battery preparation method that a kind of flexibility is filled soon |
| CN107293701A (en) * | 2016-03-31 | 2017-10-24 | 比亚迪股份有限公司 | A kind of lithium ion battery anode active material and preparation method thereof, negative pole and the lithium ion battery comprising the negative pole |
| CN107863489A (en) * | 2017-10-30 | 2018-03-30 | 周燕红 | A kind of lithium ion cell positive and the lithium ion battery using the positive pole |
| CN108155345A (en) * | 2016-12-04 | 2018-06-12 | 中国科学院大连化学物理研究所 | A kind of cathode of lithium metal secondary battery and its application |
| CN108288690A (en) * | 2017-01-09 | 2018-07-17 | 溧阳天目先导电池材料科技有限公司 | A kind of lithium solid state battery cathode and its preparation method and application |
| CN108370024A (en) * | 2015-10-08 | 2018-08-03 | 威廉马歇莱思大学 | High surface area porous carbon material as electrode |
| CN108565407A (en) * | 2018-01-09 | 2018-09-21 | 苏州氟特电池材料股份有限公司 | A kind of lithium battery electrode material and preparation method thereof |
| CN109309206A (en) * | 2017-07-26 | 2019-02-05 | 中能中科（天津）新能源科技有限公司 | Disposable lithium-battery, serondary lithium battery and preparation method thereof |
| CN109309194A (en) * | 2017-07-26 | 2019-02-05 | 中能中科（天津）新能源科技有限公司 | It is modified without cathode of lithium, preparation method and contains its lithium ion battery |
| CN109309195A (en) * | 2017-07-26 | 2019-02-05 | 中能中科（天津）新能源科技有限公司 | Containing lithium electrode, preparation method and contain the lithium ion battery of the electrode |
| CN110635116A (en) * | 2018-06-22 | 2019-12-31 | 比亚迪股份有限公司 | Lithium ion battery cathode material, preparation method thereof, cathode and lithium ion battery |
| EP3598538A4 (en) * | 2017-10-27 | 2020-06-17 | LG Chem, Ltd. | Lithium metal anode structure manufacturing method and lithium metal anode structure |
| CN114784281A (en) * | 2022-05-19 | 2022-07-22 | 清华大学山西清洁能源研究院 | Composite lithium cathode of solid-state battery, preparation method of composite lithium cathode and solid-state battery |
| CN114784287A (en) * | 2022-05-17 | 2022-07-22 | 高能时代(珠海)新能源科技有限公司 | Current collector with electrostatic shielding effect, preparation method thereof and composite lithium electrode |
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| CN104937756B (en) * | 2013-01-23 | 2018-06-22 | 东丽株式会社 | Positive active material-graphene complex particle and anode material for lithium ion battery |
| EP2950373A4 (en) * | 2013-01-23 | 2016-10-26 | Toray Industries | Positive electrode active material/graphene composite particles, and positive electrode material for lithium ion battery |
| CN104937756A (en) * | 2013-01-23 | 2015-09-23 | 东丽株式会社 | Positive electrode active material/graphene composite particles, and positive electrode material for lithium ion battery |
| CN108370024A (en) * | 2015-10-08 | 2018-08-03 | 威廉马歇莱思大学 | High surface area porous carbon material as electrode |
| CN107293701A (en) * | 2016-03-31 | 2017-10-24 | 比亚迪股份有限公司 | A kind of lithium ion battery anode active material and preparation method thereof, negative pole and the lithium ion battery comprising the negative pole |
| CN108155345B (en) * | 2016-12-04 | 2020-09-15 | 中国科学院大连化学物理研究所 | Negative electrode of lithium metal secondary battery and application thereof |
| CN108155345A (en) * | 2016-12-04 | 2018-06-12 | 中国科学院大连化学物理研究所 | A kind of cathode of lithium metal secondary battery and its application |
| CN108288690A (en) * | 2017-01-09 | 2018-07-17 | 溧阳天目先导电池材料科技有限公司 | A kind of lithium solid state battery cathode and its preparation method and application |
| CN108288690B (en) * | 2017-01-09 | 2021-06-11 | 溧阳天目先导电池材料科技有限公司 | Lithium solid-state battery cathode and preparation method and application thereof |
| CN107221709A (en) * | 2017-06-09 | 2017-09-29 | 清华大学 | The lithium metal battery preparation method that a kind of flexibility is filled soon |
| CN109309195A (en) * | 2017-07-26 | 2019-02-05 | 中能中科（天津）新能源科技有限公司 | Containing lithium electrode, preparation method and contain the lithium ion battery of the electrode |
| CN109309194A (en) * | 2017-07-26 | 2019-02-05 | 中能中科（天津）新能源科技有限公司 | It is modified without cathode of lithium, preparation method and contains its lithium ion battery |
| CN109309206A (en) * | 2017-07-26 | 2019-02-05 | 中能中科（天津）新能源科技有限公司 | Disposable lithium-battery, serondary lithium battery and preparation method thereof |
| EP3598538A4 (en) * | 2017-10-27 | 2020-06-17 | LG Chem, Ltd. | Lithium metal anode structure manufacturing method and lithium metal anode structure |
| US11228029B2 (en) | 2017-10-27 | 2022-01-18 | Lg Chem, Ltd. | Method for producing lithium metal negative electrode structure and lithium metal negative electrode structure |
| CN107863489A (en) * | 2017-10-30 | 2018-03-30 | 周燕红 | A kind of lithium ion cell positive and the lithium ion battery using the positive pole |
| CN108565407A (en) * | 2018-01-09 | 2018-09-21 | 苏州氟特电池材料股份有限公司 | A kind of lithium battery electrode material and preparation method thereof |
| CN110635116A (en) * | 2018-06-22 | 2019-12-31 | 比亚迪股份有限公司 | Lithium ion battery cathode material, preparation method thereof, cathode and lithium ion battery |
| CN114784287A (en) * | 2022-05-17 | 2022-07-22 | 高能时代(珠海)新能源科技有限公司 | Current collector with electrostatic shielding effect, preparation method thereof and composite lithium electrode |
| CN114784287B (en) * | 2022-05-17 | 2024-04-05 | 高能时代(珠海)新能源科技有限公司 | Current collector with electrostatic shielding function, preparation method thereof and composite lithium electrode |
| CN114784281A (en) * | 2022-05-19 | 2022-07-22 | 清华大学山西清洁能源研究院 | Composite lithium cathode of solid-state battery, preparation method of composite lithium cathode and solid-state battery |
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Application publication date: 20130109 |