CN102916170A - Method for preparing carbon-coated nano-particle lithium titanate electrode material - Google Patents
Method for preparing carbon-coated nano-particle lithium titanate electrode material Download PDFInfo
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- CN102916170A CN102916170A CN2012104365087A CN201210436508A CN102916170A CN 102916170 A CN102916170 A CN 102916170A CN 2012104365087 A CN2012104365087 A CN 2012104365087A CN 201210436508 A CN201210436508 A CN 201210436508A CN 102916170 A CN102916170 A CN 102916170A
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- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 66
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 65
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 61
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 38
- 239000007772 electrode material Substances 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title abstract description 6
- 239000002105 nanoparticle Substances 0.000 title abstract 3
- 238000002360 preparation method Methods 0.000 claims abstract description 37
- 239000000463 material Substances 0.000 claims abstract description 28
- 238000005245 sintering Methods 0.000 claims abstract description 26
- 239000002243 precursor Substances 0.000 claims abstract description 23
- 239000011259 mixed solution Substances 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 14
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 10
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 150000001875 compounds Chemical class 0.000 claims abstract description 5
- 239000002270 dispersing agent Substances 0.000 claims abstract description 5
- 238000001694 spray drying Methods 0.000 claims description 14
- 239000004005 microsphere Substances 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 7
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- 230000002045 lasting effect Effects 0.000 claims description 6
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 229920000954 Polyglycolide Polymers 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 239000004633 polyglycolic acid Substances 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 3
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 3
- 229940071264 lithium citrate Drugs 0.000 claims description 3
- WJSIUCDMWSDDCE-UHFFFAOYSA-K lithium citrate (anhydrous) Chemical compound [Li+].[Li+].[Li+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O WJSIUCDMWSDDCE-UHFFFAOYSA-K 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 9
- 238000007599 discharging Methods 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract 2
- 239000004215 Carbon black (E152) Substances 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 238000007873 sieving Methods 0.000 abstract 1
- 238000005507 spraying Methods 0.000 abstract 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract 1
- 239000010936 titanium Substances 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 8
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
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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
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- Inorganic Compounds Of Heavy Metals (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a method for preparing a carbon-coated nano-particle lithium titanate electrode material, wherein the method comprises the following steps of: (1), adding a lithium source compound, nano-TiO2 and macromolecular hydrocarbon into a dispersing agent to prepare into a mixed solution; (2), adjusting pH of the mixed solution obtained in the step (1) to 7.0-8.5, after continuously stirring, spraying and drying to prepare a precursor, drying in vacuum at 120 DEG C, and preparing precursor powder; and (3), sintering the precursor powder obtained in the step (2) under the protection of atmosphere, sieving through a 300-mesh sieve after cooling, and then obtaining the carbon-coated nano-particle lithium titanate material. According to the invention, the carbon-coated lithium titanate electrode material with uniform nano size and particle morphology is prepared; the electrical conductivity of lithium titanate is improved; the rate charging and discharging performances of the material are increased; therefore, the material has high specific capacity and good rate capability and cycle performance; and the preparation method disclosed by the invention is simple in process and easy for control and automatic operation and is applied to scale production.
Description
Technical field
The invention belongs to the lithium titanate electrode material technical field, be specifically related to a kind of preparation method of carbon-coated nano microballoon lithium titanate electrode material.
Background technology
Li
4Ti
5O
12Have spinel structure, theoretical embedding lithium specific capacity high (175mAh/g) is a kind of " zero strain " material, and Li+ embeds therein and to deviate from the process changes in crystal structure of material very little, so material has stable cycle performance; Higher (the 1.55V vs.Li of embedding lithium current potential
+/ Li), be higher than reduction potential (the 0.8V vs.Li of common electrolyte
+/ Li), therefore do not react with it, can not cause separating out of lithium metal, so security performance is good; Compare with material with carbon element, have higher lithium ion chemical diffusion coefficient (2 * 10
-8Cm
2/ s), Li+ migration rate therein is fast, is fit to fast charging and discharging; The characteristics that also have simultaneously anti-over-charging and Heat stability is good.
At present, Li
4Ti
5O
12The subject matter that material faces is that itself intrinsic electronic conductivity is lower by (＜10
-13S/cm), belong to insulating material; Poor conductivity makes its electrical conductivity when high rate charge-discharge obstructed, and capacity attenuation is very fast, has affected its high rate charge-discharge performance.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of carbon-coated nano microballoon lithium titanate electrode material obtains nano-scale, the uniform carbon coating of granule-morphology lithium titanate, makes it have good rate charge-discharge and cycle performance.
In order to realize above purpose, the technical solution adopted in the present invention is: a kind of preparation method of carbon-coated nano microballoon lithium titanate electrode material comprises the following steps:
1) preparation of material solution: according to mol ratio 1:1:(5～20) weighing Li source compound, nano TiO 2 and high-molecular hydrocarbons add the mixed solution that is mixed with mass fraction 5%～10% in the dispersant;
2) spray drying: regulating step 1) pH of gained mixed solution is 7.0～8.5, at 20～40 ℃ of lower insulations and the lasting 1～2h that stirs, rear spray drying makes the pre-Nano microsphere lithium titanate precursor that coats of high-molecular hydrocarbons, 120 ℃ of vacuum drying 2～4h of presoma with coating in advance obtain precursor powder;
3) sintering: with step 2) gained precursor powder carries out sintering under atmosphere protection, the control temperature is at 100～250 ℃; sintering 2～6h is warming up to 300～900 ℃, sintering 8～20h again; cross 300 mesh sieves after the cooling, namely get described carbon-coated nano microballoon lithium titanate material.
Described Li source compound is any one in lithium citrate, lithium nitrate, lithium hydroxide, the lithium carbonate.
Described high-molecular hydrocarbons is any one in polyethylene glycol, poly-propyl alcohol, the polyglycolic acid.
Dispersant is any one or the mixed liquor in deionized water, the absolute ethyl alcohol in the step 1).
Step 2) use ammoniacal liquor to regulate the pH value in.
Step 2) speed that stirs in is 300rpm.
Step 2) spray-dired temperature is 150～200 ℃ in.
Atmosphere adopts high pure nitrogen in the step 3).
Heating rate is 3～5 ℃/min in the step 3).
The spinel type lithium titanate electrode material of the present invention's preparation, molecular formula is Li
4Ti
5O
12/ C.
Affect Li
4Ti
5O
12The principal element of high rate capability has Li
4Ti
5O
12The contact area of granular size, particle and electrolyte and the conductivity of material.The carbon-coated nano microballoon lithium titanate that preparation method of the present invention obtains is the particle of nano-scale, has increased the contact area of particle and electrolyte, is conducive to Li
+Transmission and diffusion, shorten simultaneously Li
+At Li
4Ti
5O
12Migration path in the particle can guarantee the quick embedding of Li+ and deviates from the situation of high power charging-discharging, make it to have good high rate capability.
Preparation method of the present invention makes the Nano microsphere lithium titanate electrode material that even carbon coats, and titanium source and lithium source nanoscale evenly mix, by the microspheroidal lithium titanate precursor material of spray drying generation, and when high-molecular hydrocarbons coats in advance, the Li of generation
4Ti
5O
12Can keep TiO
2The size and shape of particle.The carbon-coating that coats can establishment lithium titanate crystal particles reunion, control lithium titanate crystalline size; Simultaneously, Li
4Ti
5O
12The carbon-coating of particle outside is very thin and have a lot of defectives to exist, and can be used as electric bridge, guarantees that electronics can be transferred to Li fast
+The place, do not affect again simultaneously Li
+Transmission and diffusion because carbon-coating is very thin and have a lot of defectives to exist, in addition, Li
4Ti
5O
12The reducing of particle diameter can shorten Li
+The evolving path.Synthetic Li
4Ti
5O
12/ C has excellent chemical property, especially high rate capability.
The preparation method of carbon-coated nano microballoon lithium titanate electrode material of the present invention is with lithium source, nano-TiO
2, high-molecular hydrocarbons is raw material, the pre-Nano microsphere lithium titanate precursor that coats of the high-molecular hydrocarbons of the spray drying system of employing, after carry out the mode of high temperature sintering, make nano-scale, the uniform carbon-coated nano microballoon of granule-morphology lithium titanate electrode material, improve the conductive capability of lithium titanate, improve the rate charge-discharge performance of material, make material have high specific capacity, good high rate performance and cycle performance.Preparation method's technological process of the present invention is simple, is easy to control and automation mechanized operation, is applicable to large-scale production.
Description of drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the carbon-coated nano microballoon lithium titanate of embodiment 1 preparation;
Fig. 2 is the carbon-coated nano microballoon lithium titanate of embodiment 1 preparation and the XRD diffracting spectrum of the Nano microsphere lithium titanate that Comparative Examples prepares;
Wherein (a) is Li
4Ti
5O
12, (b) be Li
4Ti
5O
12/ C;
Fig. 3 is the cycle performance figure of carbon-coated nano microballoon lithium titanate material under different multiplying of embodiment 1 preparation;
Fig. 4 is the cycle performance figure of carbon-coated nano microballoon lithium titanate material under different multiplying of embodiment 2 preparations;
Fig. 5 is the cycle performance figure of carbon-coated nano microballoon lithium titanate material under different multiplying of embodiment 3 preparations;
Fig. 6 is the cycle performance figure of Nano microsphere lithium titanate material under different multiplying of Comparative Examples preparation.
Embodiment
The invention will be further described below in conjunction with embodiment:
Embodiment 1
The preparation method of the carbon-coated nano microballoon lithium titanate electrode material of present embodiment comprises the following steps:
1) preparation of material solution: according to mol ratio 1:1:10 weighing lithium carbonate, nano-TiO
2And polyethylene glycol, add in the deionized water, be mixed with the mixed solution of mass fraction 7%;
2) spray drying: use ammoniacal liquor regulating step 1) pH of gained mixed solution is 7.0,40 ℃ of lower insulations, and with the lasting 1h that stirs of 300rpm, pass through spray dryer, 150 ℃ of spray dryings make the Nano microsphere lithium titanate precursor of coated with polyethylene glycol, the presoma that coats is in advance dried 4h in 120 ℃ of vacuum drying chambers, obtain precursor powder;
3) sintering: with step 2) gained precursor powder; in the atmosphere rotary furnace, under the high pure nitrogen protection, carry out sintering; the control temperature is at 100 ℃; sintering 6h; speed with 5 ℃/min is warming up to 600 ℃ again; sintering 20h crosses 300 mesh sieves after the cooling, namely get described carbon-coated nano microballoon lithium titanate material.
The scanning electron microscope (SEM) photograph of the carbon-coated nano microballoon lithium titanate of present embodiment preparation as shown in Figure 1.
Embodiment 2
The preparation method of the carbon-coated nano microballoon lithium titanate electrode material of present embodiment comprises the following steps:
1) preparation of material solution: according to mol ratio 1:1:5 weighing lithium citrate, nano-TiO
2With poly-propyl alcohol, add and go in the absolute ethyl alcohol, be mixed with the mixed solution of mass fraction 5%;
2) spray drying: use ammoniacal liquor regulating step 1) pH of gained mixed solution is 8.0,30 ℃ of lower insulations, and with the lasting 1.5h that stirs of 300rpm, pass through spray dryer, 180 ℃ of spray dryings make the Nano microsphere lithium titanate precursor that poly-propyl alcohol coats, the presoma that coats is in advance dried 3h in 120 ℃ of vacuum drying chambers, obtain precursor powder;
3) sintering: with step 2) gained precursor powder; in the atmosphere rotary furnace, under the high pure nitrogen protection, carry out sintering; the control temperature is at 200 ℃; sintering 2h; speed with 3 ℃/min is warming up to 900 ℃ again; sintering 8h crosses 300 mesh sieves after the cooling, namely get described carbon-coated nano microballoon lithium titanate material.
Embodiment 3
The preparation method of the carbon-coated nano microballoon lithium titanate electrode material of present embodiment comprises the following steps:
1) preparation of material solution: according to mol ratio 1:1:20 weighing lithium nitrate, nano-TiO
2And polyglycolic acid, add in the mixed liquor of deionized water and absolute ethyl alcohol, be mixed with the mixed solution of mass fraction 10%;
2) spray drying: use ammoniacal liquor regulating step 1) pH of gained mixed solution is 7.0,20 ℃ of lower insulations, and with the lasting 2h that stirs of 300rpm, pass through spray dryer, 200 ℃ of spray dryings make the Nano microsphere lithium titanate precursor that polyglycolic acid coats, the presoma that coats is in advance dried 2h in 120 ℃ of vacuum drying chambers, obtain precursor powder;
3) sintering: with step 2) gained precursor powder; in the atmosphere rotary furnace, under the high pure nitrogen protection, carry out sintering; the control temperature is at 250 ℃; sintering 4h; speed with 4 ℃/min is warming up to 300 ℃ again; sintering 14h crosses 300 mesh sieves after the cooling, namely get described carbon-coated nano microballoon lithium titanate material.
Comparative Examples
The preparation method of the Nano microsphere lithium titanate electrode material of this Comparative Examples comprises the following steps:
1) preparation of material solution: according to mol ratio 1:1 weighing lithium titanate, nano-TiO
2, add in the deionized water, be mixed with the mixed solution of mass fraction 7%;
2) spray drying: use ammoniacal liquor regulating step 1) pH of gained mixed solution is 7.0,40 ℃ of lower insulations, and with the lasting 1h that stirs of 300rpm, pass through spray dryer, 150 ℃ of spray dryings make the Nano microsphere lithium titanate precursor, presoma is dried 4h in 120 ℃ of vacuum drying chambers, obtain precursor powder;
3) sintering: with step 2) gained precursor powder carries out sintering under the high pure nitrogen protection in the atmosphere rotary furnace, the control temperature is at 100 ℃; sintering 6h, the speed with 5 ℃/min is warming up to 600 ℃, sintering 20h again; cross 300 mesh sieves after the cooling, namely get described Nano microsphere lithium titanate material.
The XRD diffracting spectrum of the carbon-coated nano microballoon lithium titanate that the Nano microsphere lithium titanate of Comparative Examples preparation and embodiment 1 prepare as shown in Figure 2, wherein (a) is Li
4Ti
5O
12, (b) be Li
4Ti
5O
12/ C, angle of diffraction and peak value are consistent, show that crystal formation is consistent, without dephasign.
Electric property to the lithium titanate electrode material of embodiment 1～3 and Comparative Examples is analyzed:
The lithium titanate electrode material of embodiment 1～3 and Comparative Examples is made into 2032 type button cells to be tested.Shown in Fig. 3～6, battery core discharges and recharges at 1.0～2.5V voltage range, charges and discharge first efficient and reaches more than 95%; 0.5C the discharge gram volume reaches more than the 168mAh/g.Battery has excellent cycle performance: 2C charges and discharge 100 Capacitance reserves of circulation more than 98% under the normal temperature; Discharge is more than 95% of 1C capacity under the 10C multiplying power.Shown in the concrete measurement result table 1:
The measurement result of the battery that the lithium titanate electrode material of table 1 embodiment 1～3 and Comparative Examples is made
Claims (9)
1. the preparation method of a carbon-coated nano microballoon lithium titanate electrode material is characterized in that: comprise the following steps:
1) preparation of material solution: according to mol ratio 1:1:(5～20) weighing Li source compound, nano TiO 2 and high-molecular hydrocarbons add the mixed solution that is mixed with mass fraction 5%～10% in the dispersant;
2) spray drying: regulating step 1) pH of gained mixed solution is 7.0～8.5, at 20～40 ℃ of lower insulations and the lasting 1～2h that stirs, rear spray drying makes the pre-Nano microsphere lithium titanate precursor that coats of high-molecular hydrocarbons, 120 ℃ of vacuum drying 2～4h of presoma with coating in advance obtain precursor powder;
3) sintering: with step 2) gained precursor powder carries out sintering under atmosphere protection, the control temperature is at 100～250 ℃; sintering 2～6h is warming up to 300～900 ℃, sintering 8～20h again; cross 300 mesh sieves after the cooling, namely get described carbon-coated nano microballoon lithium titanate material.
2. the preparation method of carbon-coated nano microballoon lithium titanate electrode material according to claim 1, it is characterized in that: described Li source compound is any one in lithium citrate, lithium nitrate, lithium hydroxide, the lithium carbonate.
3. the preparation method of carbon-coated nano microballoon lithium titanate electrode material according to claim 1 is characterized in that: described high-molecular hydrocarbons is any one in polyethylene glycol, poly-propyl alcohol, the polyglycolic acid.
4. the preparation method of carbon-coated nano microballoon lithium titanate electrode material according to claim 1 is characterized in that: dispersant is any one or the mixed liquor in deionized water, the absolute ethyl alcohol in the step 1).
5. the preparation method of carbon-coated nano microballoon lithium titanate electrode material according to claim 1 is characterized in that: step 2) the middle ammoniacal liquor adjusting pH value of using.
6. the preparation method of carbon-coated nano microballoon lithium titanate electrode material according to claim 1 is characterized in that: step 2) in the speed that stirs be 300rpm.
7. the preparation method of carbon-coated nano microballoon lithium titanate electrode material according to claim 1 is characterized in that: step 2) in spray-dired temperature be 150～200 ℃.
8. the preparation method of carbon-coated nano microballoon lithium titanate electrode material according to claim 1 is characterized in that: atmosphere employing high pure nitrogen in the step 3).
9. the preparation method of carbon-coated nano microballoon lithium titanate electrode material according to claim 1, it is characterized in that: heating rate is 3～5 ℃/min in the step 3).
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| CN106684346A (en) * | 2016-12-13 | 2017-05-17 | 苏州宇量电池有限公司 | Carbon coating method suitable for preparing electrode material by spray drying method |
| CN107221642A (en) * | 2017-06-27 | 2017-09-29 | 四川兴能新材料有限公司 | A kind of preparation method of the lithium titanate of alumina-coated |
| CN107482184A (en) * | 2017-07-14 | 2017-12-15 | 东莞市迈科科技有限公司 | A preparation method of lithium titanate negative electrode composite material for lithium ion battery |
| CN107528057A (en) * | 2017-08-31 | 2017-12-29 | 北方奥钛纳米技术有限公司 | The preparation method of carbon coating lithium titanate and carbon coating lithium titanate and application |
| CN109273705A (en) * | 2018-08-29 | 2019-01-25 | 昆明理工大学 | Method for preparing lithium ion battery lithium titanate anode material |
| CN115818704A (en) * | 2022-10-28 | 2023-03-21 | 盐城工学院 | Preparation method of novel carbon-coated micro-nano square-crystal composite lithium titanate material |
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| CN106684346A (en) * | 2016-12-13 | 2017-05-17 | 苏州宇量电池有限公司 | Carbon coating method suitable for preparing electrode material by spray drying method |
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| CN107482184A (en) * | 2017-07-14 | 2017-12-15 | 东莞市迈科科技有限公司 | A preparation method of lithium titanate negative electrode composite material for lithium ion battery |
| CN107528057A (en) * | 2017-08-31 | 2017-12-29 | 北方奥钛纳米技术有限公司 | The preparation method of carbon coating lithium titanate and carbon coating lithium titanate and application |
| CN109273705A (en) * | 2018-08-29 | 2019-01-25 | 昆明理工大学 | Method for preparing lithium ion battery lithium titanate anode material |
| CN115818704A (en) * | 2022-10-28 | 2023-03-21 | 盐城工学院 | Preparation method of novel carbon-coated micro-nano square-crystal composite lithium titanate material |
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