CN103811738A - Novel titanate capable being used as lithium ion secondary battery cathode material - Google Patents
Novel titanate capable being used as lithium ion secondary battery cathode material Download PDFInfo
- Publication number
- CN103811738A CN103811738A CN201210458249.8A CN201210458249A CN103811738A CN 103811738 A CN103811738 A CN 103811738A CN 201210458249 A CN201210458249 A CN 201210458249A CN 103811738 A CN103811738 A CN 103811738A
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- Prior art keywords
- lithium
- negative material
- strontium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- 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
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a novel titanate capable of being used as a lithium ion secondary battery cathode active material. The general formula of the active material is Li2+xSrmM1-mTi5+nN1-nO14-y, wherein M is one or the combination selected from Al, Ba, Ca, Ce, Cs, La, Mg, K, Na, Sr, Mn and Sn, N is one or the combination selected from Mn, Ti, Co, Zr and V, x is greater than or equal to 0 and is less than or equal to 0.5, m is greater than or equal to 0 and is less than or equal to 1, n is greater than or equal to 0 and less than or equal to 1, and y is greater than or equal to 0 and is less than or equal to 1. The Li+/Li operating voltage from the material is 0.8-1.45V, and the metal Li potential is low compared with a lithium titanate material; when the novel titanate is paired with lithium manganate or cobalt acid lithium, the operation voltage higher than that of a battery taking lithium titanate as a negative electrode is obtained, and the safety problem of battery short circuit due to formation of lithium dendrites caused by separation of lithium metal is solved.
Description
Technical field
The present invention relates to clean energy resource field, a kind of Novel Titanium hydrochlorate that can be used as active material for negative pole of Li-ion secondary battery and preparation method thereof is provided.
Background technology
The aggravation of the environmental problem of bringing along with energy crisis and use " fossil fuel "; secondary lithium battery is as a kind of new cleaning fuel; obtain the concern of increasing research institution and new forms of energy enterprise, national governments also strengthen the supporting dynamics to these battery research and development one after another.
At present, the range of application of secondary lithium battery is more and more wider, has successfully been applied to the fields such as mobile phone, notebook computer, electric automobile and energy storage project.Along with the check of the deep and practical application of researching and developing, graphite cathode class secondary lithium battery has also spilt cruelly a series of safety problems such as " Li dendrite " (referring to Patent Document 1CN200810141740.1).People wish to find a kind of material that can substitute graphite cathode, to avoid separating out the problem of Li dendrite.The Novel lithium secondary battery cathode material that spinel type lithium titanate has " zero strain " and long-life characteristics as one has caused people's extensive concern, it is that 1.55V(refers to Patent Document 2CN200710122074.2 to Li+/Li workbench voltage), higher than the deposition potential of lithium metal.Negative electrode active material with lithium titanate as lithium secondary battery, can successfully avoid separating out and form the potential safety hazard that Li dendrite causes, the fail safe that has improved battery due to lithium metal.
But, because lithium titanate self current potential is high, cause the full cell voltage that makes negative pole of it to decline, the battery applications scope that obtains is little, be not suitable for large-scale industry uses.
Summary of the invention
In order to overcome the Li dendrite of graphite cathode, utilize " zero strain " and the long-life characteristics of lithium titanate, avoid the problems such as the complete battery operated voltage of the high impact of negative pole self current potential simultaneously.The present invention proposes a kind of Novel Titanium hydrochlorate as lithium secondary battery cathode material.
For addressing the above problem, the technical scheme of Novel Titanium hydrochlorate of ion secondary battery cathode material lithium of the present invention and preparation method thereof is specific as follows:
A kind of lithium rechargeable battery active material, it has following general formula:
Li
2+xSr
mM
1-mTi
5+nN
1-nO
14-y，
Wherein, M is one or more the combination in Al, Ba, Ca, Ce, Cs, La, Lr, Mg, K, Na, Mn or Sn, and N is one or more the combination in Mn, Co, Zr or V, 0≤x≤0.5,0≤m≤1,0≤n≤1,0≤y≤1.
This material its to Li
+/ Li working voltage platform scope is 0.8 ~ 1.45V; Its crystal is rhombic system.
Preferably, y=0, n=1; Now in material, Sr is replaced by M part, and general formula becomes Li
2+xsr
mm
1-mti
6o
14, wherein M is one or more the combination in Al, Ba, Ca, Ce, Cs, La, Mg, K, Na, Mn or Sn, 0≤x≤0.5,0≤m≤1.
Another preferred version of the present invention is: y=0, m=1; Now, in material, Ti is replaced by N part, and general formula is Li
2+xsrTi
5+nn
1-no
14, wherein N is one or more the combination in Mn, Co, Zr or V, 0≤x≤0.5,0≤n≤1.
Preferred again, n=1, m=1; Material makes under inertia or reducing atmosphere, has general formula Li
2+xsrTi
6o
14-y, wherein inert atmosphere is N
2, Ar or its mixed atmosphere, reducing atmosphere is for containing H
2or NH
3with the gaseous mixture of inert atmosphere, 0≤x≤0.5,0≤y≤1.
In such scheme, described negative material surface can be coated with conducting metal, metal oxide or conductive carbon agent.Wherein conducting metal and metal oxide are one or more the combination in Sn, Cu, Ag or Al and their oxide, conductive carbon agent is the carbon simple substance such as graphite, Graphene, carbon nano-tube, or one or more of the Organic Compounds RESEARCH OF PYROCARBON under inertia or reducing atmosphere, or several combinations in described carbon simple substance and described RESEARCH OF PYROCARBON.
The preparation method of Novel Titanium hydrochlorate of the present invention comprises the following steps:
1) take needed raw material by each metallic element mol ratio in product, mix and be placed in atmosphere furnace, be raised to 700 degree with 5 ℃/min programming rate, be incubated 8 hours;
2) said mixture is naturally cooled to room temperature, grind, then gained powder is placed in to atmosphere furnace and is warmed up to 1000 ℃ of insulation 24h, naturally cool to room temperature and can obtain product.
Wherein, raw material is the compound of lithium compound, titanium compound, strontium compound and metallic element M, N.
Described lithium compound is one or more the combination in lithium carbonate, lithium hydroxide, lithium nitrate, lithium acetate, lithium borate or lithium chloride;
Described titanium compound is rutile titanium dioxide or anatase titanium dioxide;
Described strontium compound is one or more the combination in strontium hydroxide, strontium carbonate, strontium chloride, strontium acetate or strontium sulfate;
The compound of described metallic element M, N is one or more the combination in oxide, carbonate or the hydroxide of respective metal element.
Take above-mentioned titanate as anodal, the button cell working voltage platform scope of making take lithium metal as negative pole is 0.8～1.45V, and this value is higher than the deposition potential of lithium metal, lower than Li
4ti
5o
12(vs.Li
+/ Li) 1.55V platform.
Novel Titanium silicate material of the present invention is to Li
+/ Li operating voltage is 0.8～1.45V, compared with lithium titanate material, lower to metal Li current potential, like this when with LiMn2O4 or the pairing of cobalt acid lithium, can obtain and compare the operating voltage that the battery take lithium titanate as negative pole is higher, and can solve equally and separate out and form due to lithium metal the safety problem that Li dendrite causes battery short circuit.This material high rate performance is better, and specific area is little, embodies good processing characteristics in battery manufacturing process, and in addition, its synthesis technique is simple, and raw material cheapness is applicable to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the Novel Titanium hydrochlorate XRD spectra of the embodiment of the present invention 1;
Fig. 2 is Novel Titanium hydrochlorate electron microscope (SEM) photo of the embodiment of the present invention 1;
Fig. 3 is that the Novel Titanium hydrochlorate of the embodiment of the present invention 1 is to Li
+charging/discharging voltage-specific capacity curve of/Li.
Embodiment
Titanate the present invention being proposed below in conjunction with embodiment is described in more detail.And protection scope of the present invention is not only confined to following examples.The those of ordinary skill of described technical field, according to above disclosure of the present invention, all can be realized object of the present invention.
Embodiment mono-:
Li
2.1srTi
6o
14preparation
Selecting lithium carbonate, anatase titanium dioxide and strontium carbonate is raw material, Li:Sr:Ti=2.1:1:6 batching in molar ratio, be placed in atmosphere furnace through mixing, under air atmosphere, be raised to 700 degree with 5 ℃/min programming rate, be incubated 8 hours, then naturally cool to room temperature, after grinding, then powder is placed in to atmosphere furnace, and under air atmosphere, be warmed up to 1000 ℃ of insulation 24h, naturally cool to afterwards room temperature and can obtain faint yellow product.Fig. 1 is its X-ray diffraction collection of illustrative plates, and figure bis-is its ESEM (SEM) photo, and it is Fig. 3 to charging/discharging voltage-capacity curve of Li+/Li.
Embodiment bis-:
Li
2.1srTi
6o
14preparation
Selecting lithium carbonate, anatase titanium dioxide and strontium hydroxide is raw material, Li:Sr:Ti=2.1:1:6 batching in molar ratio, be placed in atmosphere furnace through mixing, under air atmosphere, be raised to 700 degree with 5 ℃/min programming rate, be incubated 8 hours, then naturally cool to room temperature, after grinding, then powder is placed in to atmosphere furnace, and under air atmosphere, be warmed up to 1000 ℃ of insulation 24h, naturally cool to afterwards room temperature and can obtain faint yellow product.
Embodiment tri-:
Li
2.1sr
0.98mg
0.02ti
6o
14preparation
Selecting lithium carbonate, anatase titanium dioxide, strontium carbonate and magnesium hydroxide is raw material, Li:Sr:Mg:Ti=2.1:0.98:0.02:6 batching in molar ratio, be placed in atmosphere furnace through mixing, under air atmosphere, be raised to 700 degree with 5 ℃/min programming rate, be incubated 8 hours, then naturally cool to room temperature, after grinding, then powder is placed in to atmosphere furnace, and under air atmosphere, be warmed up to 1000 ℃ of insulation 24h, naturally cool to afterwards room temperature and can obtain faint yellow product.
Embodiment tetra-:
Li
2.1srTi
5.98mn
0.02o
14preparation
Selecting lithium carbonate, anatase titanium dioxide, strontium carbonate and manganese dioxide is raw material, Li:Sr:Ti:Mn=2.1:1:5.98:0.02 batching in molar ratio, be placed in atmosphere furnace through mixing, under air atmosphere, be raised to 700 degree with 5 ℃/min programming rate, be incubated 8 hours, then naturally cool to room temperature, after grinding, then powder is placed in to atmosphere furnace, and under air atmosphere, be warmed up to 1000 ℃ of insulation 24h, naturally cool to afterwards room temperature and can obtain faint yellow product.
Embodiment five:
Li
2.1srTi
6o
13.98preparation
Selecting lithium carbonate, anatase titanium dioxide and strontium carbonate is raw material, and Li:Sr:Ti=2.1:1:6 batching in molar ratio, is placed in atmosphere furnace through mixing, and logical reducibility gas (is N
2with H
2gaseous mixture, volume ratio N
2: H
2=95:5) prepurging to oxygen content in stove is less than after 100ppm, regulating reducibility gas flow is 3L/min, and be raised to 700 degree with 5 ℃/min programming rate, be incubated 8 hours, then naturally cool to room temperature, after grinding, then powder is placed in to atmosphere furnace, under reducing atmosphere, be warmed up to 1000 ℃ of insulation 24h, naturally cool to afterwards room temperature and can obtain faint yellow product.
Embodiment six:
Carbon is coated Li
2.1srTi
6o
14preparation
Selecting lithium carbonate, anatase titanium dioxide, strontium carbonate and glucose is raw material, Li:Sr:Ti in molar ratio: glucose=2.1:1:6:0.45 batching, be placed in atmosphere furnace through mixing, logical nitrogen prepurging to oxygen content in stove is less than after 100ppm, adjusting mixed gas flow is 3L/min, be raised to 700 degree with 5 ℃/min programming rate, be incubated 8 hours, then naturally cool to room temperature, after grinding, again powder is placed in to atmosphere furnace, under nitrogen atmosphere, is warmed up to 1000 ℃ of insulation 24h, naturally cool to afterwards room temperature and can obtain grey black carbon coated product.
Claims (13)
1. a negative material for lithium rechargeable battery, is characterized in that this material has following general formula:
Li
2+xSr
mM
1-mTi
5+nN
1-nO
14-y，
Wherein, M is one or more in Al, Ba, Ca, Ce, Cs, La, Mg, K, Na, Mn or Sn, and N is one or more in Mn, Co, Zr or V, 0≤x≤0.5,0≤m≤1,0≤n≤1,0≤y≤1.
2. negative material as described in claim 1, is characterized in that Li
+/ Li voltage platform is 0.8～1.45V.
3. negative material as described in claim 1, the crystal structure that it is characterized in that this material is rhombic system.
4. negative material as described in claim 1, is characterized in that preferred y=0 in described general formula, n=1.
5. negative material as described in claim 1, it is characterized in that preferred, y=0 in general formula, m=1.
6. negative material as described in claim 1, it is characterized in that preferred, n=1 in general formula, when m=1, described negative material makes under inertia or reducing atmosphere, wherein inert atmosphere is N
2, Ar or its mixed atmosphere, reducing atmosphere is for containing H
2or NH
3gaseous mixture with inert atmosphere.
7. negative material as described in claim 1, it is characterized in that described negative material surface is coated with conducting metal, metal oxide or conductive carbon agent, wherein conducting metal and metal oxide are one or more the combination in Sn, Cu, Ag, Al and oxide thereof, conductive carbon agent is the carbon simple substance such as graphite, Graphene, carbon nano-tube, or one or more of the Organic Compounds RESEARCH OF PYROCARBON under inertia or reducing atmosphere, or several combinations in described carbon simple substance and described RESEARCH OF PYROCARBON.
8. the preparation method of the negative material as described in above arbitrary claim, is characterized in that comprising the steps:
1) take needed raw material by each metallic element mol ratio in product, mix and be placed in atmosphere furnace, be raised to 700 degree with 5 ℃/min programming rate, be incubated 8 hours;
2) said mixture is naturally cooled to room temperature, grind, then gained powder is placed in to atmosphere furnace and is warmed up to 1000 ℃ of insulation 24h, naturally cool to room temperature and can obtain product.
9. the preparation method described in claim 8, is characterized in that raw material described in step 1) is the compound of lithium compound, titanium compound, strontium compound and metallic element M, N.
10. the preparation method described in claim 9, is characterized in that described lithium compound is one or more the combination in lithium carbonate, lithium hydroxide, lithium nitrate, lithium acetate, lithium borate or lithium chloride.
Preparation method described in 11. claims 9, is characterized in that described titanium compound is the one in rutile titanium dioxide or anatase titanium dioxide.
Preparation method described in 12. claims 9, is characterized in that described strontium compound is one or more the combination in strontium hydroxide, strontium carbonate, strontium chloride, strontium acetate or strontium sulfate.
Preparation method described in 13. claims 9, the compound that it is characterized in that described metallic element M, N is one or more the combination in the oxide, carbonate, hydroxide of respective metal element.
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| CN105185972A (en) * | 2014-05-27 | 2015-12-23 | 中信国安盟固利动力科技有限公司 | Composite titanate negative electrode material of lithium ion secondary battery and synthetic method thereof |
| CN105417576A (en) * | 2014-09-23 | 2016-03-23 | 中信国安盟固利动力科技有限公司 | Preparation method for high power spherical titanate anode material |
| CN106033809A (en) * | 2015-03-17 | 2016-10-19 | 中信国安盟固利动力科技有限公司 | Composite titanium oxide negative electrode material and fast charging type lithium ion battery containing the same |
| CN106104866A (en) * | 2015-01-30 | 2016-11-09 | 株式会社东芝 | Battery component and set of cells |
| EP3136473A1 (en) * | 2015-08-25 | 2017-03-01 | Kabushiki Kaisha Toshiba | Active material, nonaqueous electrolyte battery, battery module, battery pack, automobile and vehicle |
| CN106575754A (en) * | 2014-12-02 | 2017-04-19 | 株式会社东芝 | Negative electrode active material, nonaqueous electrolyte battery and battery pack |
| EP3220457A1 (en) * | 2016-03-15 | 2017-09-20 | Kabushiki Kaisha Toshiba | Electrode active material, non-aqueous electrolyte secondary battery, battery pack, and vehicle |
| US10505186B2 (en) | 2015-01-30 | 2019-12-10 | Kabushiki Kaisha Toshiba | Active material, nonaqueous electrolyte battery, battery pack and battery module |
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| CN105185972B (en) * | 2014-05-27 | 2018-05-29 | 中信国安盟固利动力科技有限公司 | The compound titanate negative material and its synthetic method of a kind of lithium rechargeable battery |
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| EP3220457A1 (en) * | 2016-03-15 | 2017-09-20 | Kabushiki Kaisha Toshiba | Electrode active material, non-aqueous electrolyte secondary battery, battery pack, and vehicle |
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Application publication date: 20140521 |
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