CN104124447B - A kind of New Co (OH) F lithium ion battery cathode material and its preparation method - Google Patents
A kind of New Co (OH) F lithium ion battery cathode material and its preparation method Download PDFInfo
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- CN104124447B CN104124447B CN201410306176.XA CN201410306176A CN104124447B CN 104124447 B CN104124447 B CN 104124447B CN 201410306176 A CN201410306176 A CN 201410306176A CN 104124447 B CN104124447 B CN 104124447B
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- lithium ion
- ion battery
- negative material
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- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 26
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000010406 cathode material Substances 0.000 title abstract description 5
- 239000000463 material Substances 0.000 claims abstract description 19
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims abstract description 18
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229940011182 cobalt acetate Drugs 0.000 claims abstract description 9
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims abstract description 9
- 235000013024 sodium fluoride Nutrition 0.000 claims abstract description 9
- 239000011775 sodium fluoride Substances 0.000 claims abstract description 9
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims abstract description 7
- 239000004312 hexamethylene tetramine Substances 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 4
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims abstract description 4
- 239000008103 glucose Substances 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000006227 byproduct Substances 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims 1
- 235000001727 glucose Nutrition 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000010189 synthetic method Methods 0.000 abstract description 2
- 229910017052 cobalt Inorganic materials 0.000 description 5
- 239000010941 cobalt Substances 0.000 description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 5
- 239000002131 composite material Substances 0.000 description 3
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 description 2
- 229910011281 LiCoPO 4 Inorganic materials 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 1
- 229910010707 LiFePO 4 Inorganic materials 0.000 description 1
- 229910015645 LiMn Inorganic materials 0.000 description 1
- 229910018095 Ni-MH Inorganic materials 0.000 description 1
- 229910018477 Ni—MH Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- -1 ammonia radical ion Chemical class 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- OJIJEKBXJYRIBZ-UHFFFAOYSA-N cadmium nickel Chemical compound [Ni].[Cd] OJIJEKBXJYRIBZ-UHFFFAOYSA-N 0.000 description 1
- 230000004087 circulation Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
-
- 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
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
- H01M4/1315—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx containing halogen atoms, e.g. LiCoOxFy
-
- 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
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
-
- 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 kind of Novel cathode material for lithium ion battery, this negative material is shaft-like, and pole length is 1-5 μm, and diameter is 100nm-1 μm.The preparation method of described shaft-like Co (OH) F lithium ion battery negative material, it is raw material based on cobalt acetate, sodium fluoride and hexamethylenetetramine or glucose, there is chemical reaction under hydrothermal conditions, obtain shaft-like Co (OH) F lithium ion battery negative material.This negative material synthetic method is simple, is easy to operation; Gained sample is microbot shape, length 1 ~ 5 μm, diameter 100nm ~ 1 μm; Prepared material capacity is higher, has potential using value in lithium ion battery.
Description
Technical field
The present invention relates to a kind of preparation method of Novel cathode material for lithium ion battery, particularly the preparation method of the shaft-like Co of one (OH) F lithium ion battery negative material, belongs to electrochemistry field of novel.
Background technology
It is high that lithium ion battery has operating voltage, specific capacity is high, specific power is large, and charge and discharge potential curve is steady, has extended cycle life, memory-less effect, self discharge is little, advantages of environment protection, is the third generation small battery after nickel-cadmium cell, Ni-MH battery, thus notebook computer is widely used in, the Mobile portable equipments such as mobile phone.In addition, lithium ion battery is also considered to be the ideal power source of following electric vehicle.The research direction of following lithium ion battery mainly concentrates on research and development high-energy-density, high power lithium ion cell, and its key is to design and prepare the superior electrode material of high power capacity, high rate performance.At present, positive electrode is generally containing lithium transition group metallic oxide (LiCoO
2, LiFePO
4, LiMn
2o
4, LiN
1-y-zmn
yco
zo
zdeng), the feature of existing positive electrode is that charge and discharge potential is higher, and cycle performance is more stable, but specific capacity is on the low side.Traditional graphite cathode material theoretical capacity is lower, and density is lower, and volume and capacity ratio is low.Its intercalation potential is lower in addition easily causes safety problem.Thus research and develop novel high-capacity, high-performance negative material becomes and improve the effective way of capacity of lithium ion battery.Cobalt-based composite material plays an important role in the development of lithium ion battery always, such as cobalt acid lithium facilitates the development of lithium ion battery as anode material for lithium-ion batteries, becomes main positive electrode within a very long time.And the cobalt-based composite material of other kind, as LiCoPO
4, LiCoPO
4f, LiCoSO
4f, LiCoSO
4oH, CoCO
3and Co
2snO
4deng also showing good chemical property.Therefore, develop straightforward procedure preparation there is the novel cobalt-based composite material of special appearance and structure and study its chemical property and have great importance.Up to the present, about the Electrochemical Properties of Co (OH) F material, there is not been reported.Based on above background, invention one prepares the new method of shaft-like Co (OH) F material, has shown obviously charge and discharge platform using it as lithium ion battery negative, shows that it has potential using value in lithium ion battery.
Summary of the invention
To the object of the invention is to cobalt acetate, sodium fluoride and hexamethylenetetramine or glucose, for raw material, prepare shaft-like lithium ion battery negative material Co (OH) F by hydro thermal method.Its principle is exactly the high temperature utilized under hydrothermal condition, hyperbaric environment promotes chemical reaction process in solution, thus prepares good shaft-like Co (OH) F of crystal property.
Co (OH) F synthesis material involved in the present invention is cobalt acetate, sodium fluoride and hexamethylenetetramine.In material preparation process, first cobalt acetate, sodium fluoride and hexamethylenetetramine are taken by a certain percentage, be positioned over adding distil water in beaker and stir, be then transferred in hydrothermal reaction kettle in 120 DEG C ~ 180 DEG C reactions 12 ~ 48 hours.Product is centrifugal, dry, collect.
Co (OH) F negative material involved in the present invention and preparation method have following outstanding feature:
(1) the present invention utilize hexamethylenetetramine under hydrothermal conditions slow releasing ammonia radical ion provide alkaline environment for solution, promote that chemical reaction occurs.
(2) synthetic method is simple, is easy to operation.
(3) gained sample is microbot shape, length 1 ~ 5 μm, diameter 100nm ~ 1 μm.
(4) prepared material capacity is higher, has potential application in lithium ion battery.
accompanying drawing illustrates:
The XRD collection of illustrative plates of sample prepared by Fig. 1 embodiment 1.
The SEM figure of sample prepared by Fig. 2 embodiment 1.
Charge and discharge curve (a) first of sample prepared by Fig. 3 embodiment 1 and cycle performance figure (b).
The XRD collection of illustrative plates of sample prepared by Fig. 4 embodiment 2.
The SEM collection of illustrative plates of sample prepared by Fig. 5 embodiment 2.
The XRD collection of illustrative plates of sample prepared by Fig. 6 embodiment 3.
embodiment:
Embodiment 1
By cobalt acetate, sodium fluoride and hexamethylenetetramine in molar ratio for 1:1:5 takes, be positioned over adding distil water in beaker to stir, be transferred in hydro-thermal axe and react 24 hours at 120 DEG C, by product alcohol, distilled water eccentric cleaning, be transferred in culture dish and dry derived sample.Result shows, prepared sample, through XRD atlas analysis, is positioned at 20.9 °, 32.3 °, 33.5 °, 34.7 °, 35.6 °, 38.8 °, 39.9 °, 43.6 °, 51.9 °, 52.8 °, 56.9 °, 59.1 ° and 61.6
othe diffraction maximum at place and (110) of rhombic system Co (OH) F, (310), (201), (400), (111), (211), (410), (311), (221), (420), (511), (002) and (601) crystal face corresponding, with XRD card JCPDS, no.50-0827 is consistent.Prepared sample characterizes through SEM, and as shown in Fig. 2 (a), be made up of a large amount of microbot, its distribution of lengths is 1 ~ 5 μm.From Fig. 2 (b), the diameter of microbot is distributed as between 100nm ~ 1 μm.As the curve of charge and discharge first and cycle performance that Fig. 3 is prepared shaft-like lithium ion battery negative material Co (OH) F, its charge and discharge specific capacity is first respectively 661.1,992mAh/g, after 40 circulations charge and discharge capacity be respectively 330.1,332.8mAh/g, show that it has potential using value in lithium ion battery.
Embodiment 2
By cobalt acetate, sodium fluoride and glucose 1:1 in molar ratio; 1 takes, and is positioned over adding distil water in beaker and stirs, and is transferred in hydro-thermal axe and reacts 24 hours in 120 DEG C, by product alcohol, distilled water eccentric cleaning, be transferred in culture dish and dry derived sample.Show through XRD atlas analysis, as shown in Figure 4, gained sample main component is still Co (OH) F(JCPDS, the no.50-0827 of rhombic system), the diffraction maximum being positioned at 23 ° and 46.7 ° places shows that prepared sample contains the hydrocarbon impurity of a small amount of cobalt.Prepared sample characterizes through SEM, as shown in Fig. 5 (a), is made up of a large amount of irregular particle.From Fig. 5 (b), the average-size of particle is about 500nm.
Embodiment 3
Cobalt acetate and sodium fluoride are taken by 1:1, is positioned over adding distil water in beaker and stirs, be transferred in hydro-thermal axe and react 24 hours in 120 DEG C, by product alcohol, distilled water eccentric cleaning, be transferred in culture dish and dry derived sample.Show through XRD atlas analysis, as shown in Figure 6, gained sample is NaCoF
4and NaCoF
3mixture.
Claims (2)
1. the preparation method of Co (OH) F lithium ion battery negative material, it is characterized in that: by cobalt acetate, sodium fluoride and hexamethylenetetramine in molar ratio for 1:1:5 takes, be positioned over adding distil water in beaker to stir, be transferred in water heating kettle and react 24 hours at 120 DEG C, by product alcohol, distilled water eccentric cleaning, be transferred in culture dish to dry and can obtain shaft-like Co (OH) F lithium ion battery negative material, pole length is 1-5 μm, and diameter is 100nm-1 μm.
2. the preparation method of Co (OH) F lithium ion battery negative material, it is characterized in that: by cobalt acetate, sodium fluoride and glucose in molar ratio 1:1:1 take, be positioned over adding distil water in beaker to stir, be transferred in hydro-thermal axe in 120 DEG C of reactions 24 hours, by product alcohol, distilled water eccentric cleaning, be transferred in culture dish to dry and can obtain granular Co (OH) F lithium ion battery negative material, the average-size of particle is 500nm.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410306176.XA CN104124447B (en) | 2014-07-01 | 2014-07-01 | A kind of New Co (OH) F lithium ion battery cathode material and its preparation method |
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| CN201410306176.XA CN104124447B (en) | 2014-07-01 | 2014-07-01 | A kind of New Co (OH) F lithium ion battery cathode material and its preparation method |
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| CN104124447A CN104124447A (en) | 2014-10-29 |
| CN104124447B true CN104124447B (en) | 2016-03-16 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104993105B (en) * | 2015-05-27 | 2018-05-08 | 三峡大学 | A kind of Zinc-base compounded material fluorination zinc hydroxide and its preparation method and application |
| CN107265518B (en) * | 2017-07-04 | 2019-03-29 | 北京科技大学 | A kind of lithium ion battery negative material Co (OH) F and preparation method with Magen David structure |
| CN108467068B (en) * | 2018-03-26 | 2020-08-04 | 宁夏大学 | Cox(OH)yPreparation method and application of M |
| CN110354875B (en) * | 2019-05-24 | 2021-05-07 | 深圳欧赛技术有限公司 | Yttrium-phosphorus-codoped Co (OH) F loaded on surface of foamed nickel and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102556941A (en) * | 2012-01-05 | 2012-07-11 | 浙江大学 | Cobaltosic oxide nanowire array, preparation method thereof as well as application of nanowire array as cathode of lithium ion battery |
| CN103543184A (en) * | 2013-10-18 | 2014-01-29 | 浙江大学 | Gas-sensitive sensor based on cobaltosic oxide nanoneedle as well as preparation method thereof |
-
2014
- 2014-07-01 CN CN201410306176.XA patent/CN104124447B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102556941A (en) * | 2012-01-05 | 2012-07-11 | 浙江大学 | Cobaltosic oxide nanowire array, preparation method thereof as well as application of nanowire array as cathode of lithium ion battery |
| CN103543184A (en) * | 2013-10-18 | 2014-01-29 | 浙江大学 | Gas-sensitive sensor based on cobaltosic oxide nanoneedle as well as preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 0.11H2O and Their Electrochemical Properties".《The Journal of Physical Chemistry C》.2013,第117卷第20465-20473页. * |
| Liping Zhu 等."Porous CoO Nanostructure Arrays Converted from Rhombic Co(OH)F and Needle-like Co(CO3)0.5(OH)• * |
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