CN104393272A - Lithium titanate cathode composite material and preparation method - Google Patents
Lithium titanate cathode composite material and preparation method Download PDFInfo
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- CN104393272A CN104393272A CN201410569303.5A CN201410569303A CN104393272A CN 104393272 A CN104393272 A CN 104393272A CN 201410569303 A CN201410569303 A CN 201410569303A CN 104393272 A CN104393272 A CN 104393272A
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- H01M4/362—Composites
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- 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 lithium titanate cathode composite material and a preparation method thereof. The preparation method comprises the following steps: completely dispersing a nanocarbon material in a solvent to prepare a nanocarbon sizing agent; respectively weighing a lithium compound and a titanium compound according to the proportion that the molar ratio of the lithium element to the titanium element is (3.5-4.5):5, adding into the prepared nanocarbon sizing agent, and fully mixing to obtain a precursor sizing agent; carrying out spray drying granulation on the precursor sizing agent to obtain precursor powder; sintering the precursor powder at 800-900 DEG C for 1-10 h, and cooling to obtain the lithium titanate cathode composite material. The prepared lithium titanate/nanocarbon composite material can enhance the capacity of the high-rate lithium titanate active material, and improves the energy density of electrodes.
Description
Technical field
The present invention relates to a kind of lithium titanate class anode material and preparation method, belong to nanometer and chemical materials preparation field.
Background technology
The subject matter that lithium-ion-power cell exists at present is that quick charge and security performance are poor.Compared with graphite cathode, lithium titanate anode can significantly improve quick charge and the security performance of lithium-ion-power cell, has larger application prospect.But lithium titanate material conductivity is extremely low, make lithium titanate electric conductivity very poor, become one of bottleneck of its application to a certain extent.
For improving the electric conductivity of lithium titanate anode material, currently used method mainly contains three kinds: prepare nano lithium titanate, reduces its particle diameter to shorten lithium ion the evolving path, thus improves conductivity; Doping; Carbon is coated.Wherein, carbon coating technology mainly passes through in lithium titanate particle Surface coating conductive carbon layer, to improve the electric conductivity of material.
CN 102130324 A discloses a kind of preparation method of lithium titanate/carbon nano tube composite cathode material, is wherein to be dissolved in by the compound of titanium in absolute ethyl alcohol as A liquid; Being dissolved by lithium compound and add CNT (carbon nano-tube) afterwards in deionized water and add absolute ethyl alcohol, is B liquid; After stirring, in B liquid, add appropriate organic acid, continue to stir; Slowly add in A liquid by B liquid under magnetic stirring, aging 1 ~ 12 hour is C liquid; In vacuum drying chamber, dry C liquid makes it become xerogel, then 250 ~ 450 DEG C of presintering 1 ~ 4 hour under nitrogen atmosphere, then 600 ~ 1200 DEG C of sintering 4 ~ 12 hours, product was through grinding and obtaining lithium titanate/carbon nano tube composite cathode material.The specific capacity of this material under 0.1C when the 50th week can reach 171mAhg
-1.
CN 102496707 A discloses a kind of preparation method of nano-grade-carbon-clad spinel lithium titanate battery cathode material, is wherein to put in dispersant by titanium dioxide and lithium source, Homogeneous phase mixing post-drying; By the mixture after drying under the first atmosphere with the temperature preroast 2 ~ 36 hours of 400 ~ 800 DEG C, then naturally cool to room temperature, acquisition intermediate product; Obtained intermediate product and carbon source are put in dispersant, Homogeneous phase mixing post-drying; By the mixture of intermediate product, carbon source and dispersant after drying under the second atmosphere with the temperature after baking 2 ~ 36 hours of 700 ~ 950 DEG C, naturally cool to room temperature, acquisition nano-carbon coated spinel lithium titanate.
CN 102646810 A discloses the preparation method of a kind of three-dimensional porous Graphene doping and coated lithium titanate composite anode material, wherein three-dimensional porous Graphene is dissolved in solvent be made into 1-12mg/mL solution, add Li source compound under agitation, titanium source compound, the mol ratio of control Li atom and Ti atom is (0.7 ~ 0.9): 1, obtain three-dimensional porous Graphene and lithium titanate precursor collosol and gel, three-dimensional porous Graphene and lithium titanate precursor collosol and gel are dry except desolventizing under 70 ~ 90 DEG C of conditions, obtain three-dimensional porous Graphene and lithium titanate precursor powder, under inert gas shielding, three-dimensional porous Graphene and lithium titanate precursor powder are heated to 700 ~ 950 DEG C and continue 8 ~ 20 hours, namely obtain the doping of three-dimensional porous Graphene and coated lithium titanate composite material, three-dimensional porous Graphene doping is 1 ~ 5wt% with the mass percent of three-dimensional porous Graphene in coated lithium titanate composite material.
The above-mentioned method preparing carbon coated lithium titanate class negative material, technique is comparatively complicated, is unfavorable for large-scale industrial production.
Summary of the invention
Main purpose of the present invention is the preparation method providing a kind of lithium titanate class anode material; by simple technique; preparation has comparatively small particle diameter size, the uniform titanium negative electrode composite material for lithium of granule-morphology; improve the electric conductivity of lithium titanate anode material, and be suitable for large-scale production.
Another object of the present invention is to provide the lithium titanate class prepared according to described method anode material.
For reaching above-mentioned purpose, on the one hand, the invention provides a kind of preparation method of lithium titanate class anode material, the method comprises:
(1) nano-carbon material is fully disperseed in a solvent, prepare the slurry of nano-sized carbon;
(2) ratio being 3.5 ~ 4.5:5 according to elemental lithium and titanium elements mol ratio takes lithium-containing compound and titanium-containing compound respectively, is joined in the slurry of the obtained nano-sized carbon of step (1), fully mixes, obtain precursor pulp;
(3) precursor pulp that step (2) obtains is carried out spray drying granulation, obtain presoma powder;
(4) presoma powder step (3) obtained, in 800 ~ 900 DEG C of roastings 1 ~ 10 hour, namely obtains described lithium titanate class anode material after cooling.
According to specific embodiment of the invention scheme, in the preparation method of lithium titanate class anode material of the present invention, when preparing the slurry of nano-sized carbon, described solvent is deionized water, nitrogen methyl pyrrolidone or isopropyl alcohol.
According to specific embodiment of the invention scheme, in the preparation method of lithium titanate class anode material of the present invention, described nano-sized carbon comprise in carbon nano-fiber, carbon nano-tube, Graphene and nano carbon black (conductive black) one or more.These nano-carbon materials all have high electrical conductivity.
According to specific embodiment of the invention scheme, in the preparation method of lithium titanate class anode material of the present invention, the slurry solid holdup of the nano-sized carbon that step (1) is obtained is 1 ~ 5%.
According to specific embodiment of the invention scheme, in the preparation method of lithium titanate class anode material of the present invention, in step (1), fluid dispersion technology is adopted to the dispersion of nano-sized carbon.Preferably, fluid dispersion technology of the present invention carries out high speed shear dispersion under 5000-20000rpm rotating speed.Common shearing jitter time is 5 minutes to 2 hours.
According to specific embodiment of the invention scheme, in the preparation method of lithium titanate class anode material of the present invention, described lithium-containing compound comprise in lithium hydroxide, lithium carbonate and lithium acetate one or more; Described titanium-containing compound comprise in titanium dioxide, titanium chloride and tetrabutyl titanate one or more.
According to specific embodiment of the invention scheme, in the preparation method of lithium titanate class anode material of the present invention, in described lithium titanate class anode material, the mass percentage of lithium titanate is 40 ~ 94%, is preferably 80 ~ 94%.
According to specific embodiment of the invention scheme, in the preparation method of lithium titanate class anode material of the present invention, well-mixed for the slurry of lithium-containing compound, titanium-containing compound and nano-sized carbon being operating as is stirred.Be preferably and stir 10 minutes to 1 hour under 100 ~ 500rpm rotating speed.
According to specific embodiment of the invention scheme, in the preparation method of lithium titanate class anode material of the present invention, in step (3), the temperature of spray drying granulation is 260 ~ 350 DEG C.
According to specific embodiment of the invention scheme, in the preparation method of lithium titanate class anode material of the present invention, the roasting time of presoma powder is 1 ~ 10 hour, and roasting time depends primarily on titanium source used and lithium source.
On the other hand, present invention also offers a kind of lithium titanate class anode material, it prepares according to the method described above.It has comparatively small particle diameter size, and granule-morphology is even.Electrode material of the present invention is primarily of lithium titanate and nano-sized carbon composition.Through electro-chemical test, demonstrate excellent capacity and high rate performance and good stable circulation performance.
In sum, the invention provides a kind of lithium titanate class anode material and preparation method thereof, the present invention is by directly mixing the compound containing elemental lithium, titanium elements and nano-carbon material according to special ratios, then liquid phase fluid dispersion technology is utilized to obtain uniform mixed slurry, carry out spraying dry and obtain precursor powder, the powder of gained is placed in inert gas, obtained lithium titanate/the nano carbon composite material of calcining, the load capacity of high magnification lithium titanate active material can be strengthened, improve the energy density of electrode.
Accompanying drawing explanation
Fig. 1 is the pattern under the Scanning Electron microscope of lithium titanate composite material in embodiment 1.
Fig. 2 is the X-ray diffractogram of lithium titanate composite material in embodiment 1.
Fig. 3 is the high rate performance of lithium titanate composite material under different current density in embodiment 1.
Fig. 4 is the stable circulation performance of lithium titanate composite material under the current density of 10C in embodiment 1.
Embodiment
Below by the technique effect that specific embodiment further describes feature of the present invention and has, but the present invention is not therefore subject to any restriction.
Embodiment 1
Carbon nano-tube is added in isopropanol solvent, utilizes high-velocity fluid separating apparatus 10000rpm to carry out fully dispersion 30 minutes, prepare solid holdup 1% slurry.Then the ratio being 4.2:5 according to elemental lithium and titanium elements mol ratio takes a certain amount of lithium acetate and tetrabutyl titanate respectively, make lithium titanate at the mass percentage of composite material 89%, then joined in electrocondution slurry, stirred 30 minutes under 200rpm rotating speed to be fully mixed to get uniform presoma reaction material.By the compound obtained, be delivered to spray dryer, at 280 DEG C, carry out granulation, obtain presoma powder.The presoma powder powder obtained is put into high temperature kiln roasting, sintering temperature 800 DEG C, the time is 10 hours, just obtains the lithium titanate composite material of modification after cooling.Morphology characterization is carried out to obtained powder body material, as shown in Figure 1, under Scanning Electron microscope, can Powdered particulate material be seen, and granular materials on can see fibrous carbon nano-tube.Carry out XRD structural characterization to this powder body material further, as shown in Figure 2, relevant diffraction maximum confirms that this powder body material is lithium titanate composite material.
Obtained lithium titanate composite material is added nitrogen methyl pyrrolidone (NMP) with acetylene black and binding agent (PVDF) by 80:10:10 mass ratio mix well, obtained electrode slice, and drying 12 hours at 120 DEG C in vacuum drying oven.Making work electrode with above-mentioned electrode slice, is to electrode with metal lithium sheet, and polypropylene film is barrier film, 1mol/L LiPF
6eC+DEC (1:1, volume ratio) solution make electrolyte, in the glove box of argon gas, be assembled into button cell.Under normal temperature, carry out constant current charge-discharge loop test at LAND battery test system, the high rate performance result as Fig. 3 shows that the electrochemistry capacitance of this lithium titanate anode of the present invention under 1C reaches 170mAh g
-1, under 100C, capacity can get at 108mAh g
-1.The cyclical stability test result of Fig. 4 shows, the cyclical stability retention of 6000 circles is 98%, and this embodies the chemical property of this composite material excellence.
Embodiment 2
By carbon nano-fiber and conductive black according to mass percent 1:2, add in nitrogen methyl pyrrolidone solvent, utilize high-velocity fluid separating apparatus 20000rpm to carry out fully dispersion 5 minutes, prepare solid holdup 1% slurry.Then the ratio being 3.5:5 according to elemental lithium and titanium elements mol ratio takes a certain amount of lithium carbonate and titanium dioxide respectively, make lithium titanate at the mass percentage of composite material 90%, then joined in electrocondution slurry, stirred 10 minutes under 500rpm rotating speed to be fully mixed to get uniform presoma reaction material.By the compound obtained, be delivered to spray dryer, at 280 DEG C, carry out granulation, obtain presoma powder.The presoma powder powder obtained is put into high temperature kiln roasting, sintering temperature 800 DEG C, the time is 5 hours, just obtains the lithium titanate composite material of modification after cooling.
Then the electrode preparation method with reference to embodiment 1 prepares electrode, and through constant current charge-discharge test, result shows that the electrochemistry capacitance of this lithium titanate anode of the present invention under 1C reaches 158mAh g
-1, under 100C, capacity can get at 84mAh g
-1, the cyclical stability retention of 6000 circles is 99%.
Embodiment 3
By graphene powder and conductive black according to mass percent 1:2, add in nitrogen methyl pyrrolidone solvent, under utilizing high-velocity fluid separating apparatus 8000rpm rotating speed, carry out fully dispersion 30 minutes, prepare solid holdup 1% slurry.Then the ratio being 4.5:5 according to elemental lithium and titanium elements mol ratio takes a certain amount of lithium hydroxide and tetrabutyl titanate respectively, make lithium titanate at the mass percentage of composite material 94%, then joined in electrocondution slurry, stirred 30 minutes under 200rpm rotating speed to be fully mixed to get uniform presoma reaction material.By the compound obtained, be delivered to spray dryer, at 280 DEG C, carry out granulation, obtain presoma powder.The presoma powder powder obtained is put into high temperature kiln roasting, sintering temperature 800 DEG C, the time is 5 hours, just obtains the lithium titanate composite material of modification after cooling.
Then the electrode preparation method with reference to embodiment 1 prepares electrode, and through constant current charge-discharge test, result shows that the electrochemistry capacitance of this lithium titanate anode of the present invention under 1C reaches 165mAh g
-1, under 100C, capacity can get at 76mAh g
-1, the cyclical stability retention of 6000 circles is 98%.
Embodiment 4
By carbon nano-tube and conductive black according to mass percent 1:2, add deionized water (H to
2o) solvent, utilizes high-velocity fluid separating apparatus 15000rpm to carry out fully dispersion 30 minutes, prepare solid holdup 5% slurry.Then the ratio being 4:5 according to elemental lithium and titanium elements mol ratio takes a certain amount of lithium hydroxide and titanium dioxide respectively, make lithium titanate at the mass percentage of composite material 80%, then joined in electrocondution slurry, stirred 1 hour under 150rpm rotating speed to be fully mixed to get uniform presoma reaction material.By the compound obtained, be delivered to spray dryer, at 280 DEG C, carry out granulation, obtain presoma powder.The presoma powder powder obtained is put into high temperature kiln roasting, sintering temperature 900 DEG C, the time is 2 hours, just obtains the lithium titanate composite material of modification after cooling.
Then the electrode preparation method with reference to embodiment 1 prepares electrode, and through constant current charge-discharge test, result shows that the electrochemistry capacitance of this lithium titanate anode of the present invention under 1C reaches 175mAh g
-1, under 100C, capacity can get at 110mAh g
-1, the cyclical stability retention of 6000 circles is 100%.
Embodiment 5
Carbon nano-fiber is added in nitrogen methyl pyrrolidone solvent, utilizes high-velocity fluid separating apparatus 10000rpm to carry out fully dispersion 20 minutes, prepare solid holdup 1% slurry.Then the ratio being 4:5 according to elemental lithium and titanium elements mol ratio takes a certain amount of lithium carbonate and tetrabutyl titanate respectively, make lithium titanate at the mass percentage of composite material 89%, then joined in electrocondution slurry, stirred 30 minutes under 200rpm rotating speed to be fully mixed to get uniform presoma reaction material.By the compound obtained, be delivered to spray dryer, at 280 DEG C, carry out granulation, obtain presoma powder.The presoma powder powder obtained is put into high temperature kiln roasting, sintering temperature 900 DEG C, the time is 5 hours, just obtains the lithium titanate composite material of modification after cooling.
Then the electrode preparation method with reference to embodiment 1 prepares electrode, and through constant current charge-discharge test, result shows that the electrochemistry capacitance of this lithium titanate anode of the present invention under 1C reaches 168mAh g
-1, under 100C, capacity can get at 101mAh g
-1, the cyclical stability retention of 6000 circles is 94%.
Claims (9)
1. a preparation method for lithium titanate class anode material, the method comprising the steps of:
(1) nano-carbon material is fully disperseed in a solvent, prepare the slurry of nano-sized carbon;
(2) ratio being 3.5 ~ 4.5:5 according to elemental lithium and titanium elements mol ratio takes lithium-containing compound and titanium-containing compound respectively, is joined in the slurry of the obtained nano-sized carbon of step (1), fully mixes, obtain precursor pulp;
(3) precursor pulp that step (2) obtains is carried out spray drying granulation, obtain presoma powder;
(4) presoma powder step (3) obtained, in 800 ~ 900 DEG C of roastings 1 ~ 10 hour, namely obtains described lithium titanate class anode material after cooling.
2. the preparation method of lithium titanate class anode material according to claim 1, wherein, described nano-sized carbon comprise in carbon nano-fiber, carbon nano-tube, Graphene and nano carbon black one or more; Described solvent is deionized water, nitrogen methyl pyrrolidone or isopropyl alcohol.
3. the preparation method of lithium titanate class anode material according to claim 1, wherein, the slurry solid holdup of the nano-sized carbon that step (1) is obtained is 1 ~ 5%.
4. the preparation method of lithium titanate class anode material according to claim 1, wherein, adopts fluid dispersion technology to the dispersion of nano-sized carbon in step (1); Preferably, fluid dispersion technology carries out high speed shear dispersion under 5000 ~ 20000rpm rotating speed; Jitter time is between 5 minutes to 2 hours.
5. the preparation method of lithium titanate class anode material according to claim 1, wherein, described lithium-containing compound comprise in lithium hydroxide, lithium carbonate and lithium acetate one or more; Described titanium-containing compound comprise in titanium dioxide, titanium chloride and tetrabutyl titanate one or more.
6. the preparation method of lithium titanate class anode material according to claim 1, wherein, in described lithium titanate class anode material, the mass percentage of lithium titanate is 40 ~ 94%, is preferably 80 ~ 94%.
7. the preparation method of lithium titanate class anode material according to claim 1, wherein, stirs well-mixed for the slurry of lithium-containing compound, titanium-containing compound and nano-sized carbon being operating as.
8. the preparation method of lithium titanate class anode material according to claim 1, wherein, in step (3), the temperature of spray drying granulation is 260 ~ 350 DEG C.
9. a lithium titanate class anode material, it prepares according to the preparation method described in any one of claim 1 ~ 8.
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| CN104916843A (en) * | 2015-04-20 | 2015-09-16 | 洛阳月星新能源科技有限公司 | Natural graphite modification method for lithium ion battery negative electrode material |
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| CN105529449A (en) * | 2016-01-29 | 2016-04-27 | 珠海银隆新能源有限公司 | Lithium titanate electrode material and preparation method thereof |
| CN105702925A (en) * | 2016-01-29 | 2016-06-22 | 珠海银隆新能源有限公司 | Lithium titanate electrode material and preparation method therefor |
| CN106129394A (en) * | 2016-08-26 | 2016-11-16 | 深圳博磊达新能源科技有限公司 | A kind of lithium titanate anode material and lithium titanate battery |
| CN106129394B (en) * | 2016-08-26 | 2019-08-23 | 深圳博磊达新能源科技有限公司 | A kind of lithium titanate anode material and lithium titanate battery |
| CN106299302A (en) * | 2016-09-27 | 2017-01-04 | 深圳复兴新能源科技有限公司 | A kind of preparation method of lithium titanate anode material |
| CN107331869A (en) * | 2017-01-21 | 2017-11-07 | 深圳市瑞能达科技有限公司 | It is a kind of to lift the compound additive of lithium titanate electric material cryogenic property |
| CN106848251A (en) * | 2017-03-15 | 2017-06-13 | 北京朗盛特耐科技有限公司 | A kind of preparation method of CNT lithium titanate composite anode material |
| CN109599536A (en) * | 2017-09-30 | 2019-04-09 | 天津大学 | Germanium hydrogen/redox graphene/conductive black nano composite lithium ion cell negative electrode material and preparation method thereof |
| CN110247026A (en) * | 2018-03-08 | 2019-09-17 | 天津大学 | A kind of GeCH3-RGO-SP nano composite lithium ion cell negative electrode material and preparation method |
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