CN115974175A - Preparation method, product and application of silicon dioxide coated ternary material - Google Patents
Preparation method, product and application of silicon dioxide coated ternary material Download PDFInfo
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- CN115974175A CN115974175A CN202211588846.2A CN202211588846A CN115974175A CN 115974175 A CN115974175 A CN 115974175A CN 202211588846 A CN202211588846 A CN 202211588846A CN 115974175 A CN115974175 A CN 115974175A
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- 239000000463 material Substances 0.000 title claims abstract description 37
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 17
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 24
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- 239000002243 precursor Substances 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- MLAOBUNVZFBLLT-UHFFFAOYSA-N nickel propan-2-ol Chemical compound [Ni].CC(C)O.CC(C)O MLAOBUNVZFBLLT-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000725 suspension Substances 0.000 claims abstract description 10
- 229910003002 lithium salt Inorganic materials 0.000 claims abstract description 8
- 159000000002 lithium salts Chemical class 0.000 claims abstract description 8
- 150000001868 cobalt Chemical class 0.000 claims abstract description 7
- 150000002696 manganese Chemical class 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001354 calcination Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- UQMOLLPKNHFRAC-UHFFFAOYSA-N tetrabutyl silicate Chemical compound CCCCO[Si](OCCCC)(OCCCC)OCCCC UQMOLLPKNHFRAC-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 5
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 10
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 4
- 229940011182 cobalt acetate Drugs 0.000 claims description 4
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 4
- PFQLIVQUKOIJJD-UHFFFAOYSA-L cobalt(ii) formate Chemical compound [Co+2].[O-]C=O.[O-]C=O PFQLIVQUKOIJJD-UHFFFAOYSA-L 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 229910052744 lithium Inorganic materials 0.000 claims description 4
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 claims description 4
- XKPJKVVZOOEMPK-UHFFFAOYSA-M lithium;formate Chemical compound [Li+].[O-]C=O XKPJKVVZOOEMPK-UHFFFAOYSA-M 0.000 claims description 4
- 229940071125 manganese acetate Drugs 0.000 claims description 4
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 4
- BHVPEUGTPDJECS-UHFFFAOYSA-L manganese(2+);diformate Chemical compound [Mn+2].[O-]C=O.[O-]C=O BHVPEUGTPDJECS-UHFFFAOYSA-L 0.000 claims description 4
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 3
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 3
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 3
- 229940099607 manganese chloride Drugs 0.000 claims description 3
- 235000002867 manganese chloride Nutrition 0.000 claims description 3
- 239000011565 manganese chloride Substances 0.000 claims description 3
- 239000007774 positive electrode material Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims 1
- 238000005260 corrosion Methods 0.000 abstract description 4
- 230000007797 corrosion Effects 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000010405 anode material Substances 0.000 description 3
- 239000010406 cathode material Substances 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 229910013716 LiNi Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- JEMUNLMELOOTDQ-UHFFFAOYSA-J [Cl-].[Cl-].[Cl-].[Cl-].[Mn++].[Mn++] Chemical compound [Cl-].[Cl-].[Cl-].[Cl-].[Mn++].[Mn++] JEMUNLMELOOTDQ-UHFFFAOYSA-J 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- GHGNQWNTEPHORR-UHFFFAOYSA-L cobalt;dichlorocobalt Chemical compound [Co].Cl[Co]Cl GHGNQWNTEPHORR-UHFFFAOYSA-L 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229940071257 lithium acetate Drugs 0.000 description 1
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Images
Classifications
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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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- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention provides a preparation method of a silicon dioxide coated ternary material, a product and application thereof, wherein nickel isopropoxide and tetrabutyl silicate are dissolved in absolute ethyl alcohol for ultrasonic dispersion and stirring; dropwise adding deionized water into the suspension to form sol; adding lithium salt, cobalt salt and manganese salt into the sol, continuously stirring for 1 to 2 hours, adding into a reaction kettle, and reacting for 10 to 15 hours at 160 to 180 ℃ to obtain SiO 2 Washing the coated ternary precursor with deionized water, and vacuum-dryingDrying in an oven; mixing SiO 2 Calcining the coated ternary precursor at 600 to 800 ℃ for 3 to 5 hours to obtain SiO 2 A coated ternary material. Coated SiO 2 Prevent HF from dissolving metal elements on the surface of the material and SiO 2 Can react with a small amount of HF, reduces the corrosion of the HF on the surface of the electrode by consuming the HF, reduces the generation of impurity gas, blocks the subsequent undesirable chain reaction, and further improves the electrochemical performance of the material.
Description
Technical Field
The invention relates to a preparation method of a lithium battery anode material, in particular to a preparation method of a silicon dioxide coated ternary material, a product and application.
Background
Lithium ion secondary batteries have been widely used as high specific energy chemical power sources in the fields of mobile communication, notebook computers, video cameras, portable instruments and meters, and the like, and have rapidly developed into one of the most important secondary batteries at present. Lithium ion batteries, which are the latest generation of green high-energy storage batteries, have been rapidly developed in the early 90 s of the 20 th century, and are favored because of their advantages of high voltage, high energy density, long cycle life, little environmental pollution, and the like.
Due to the ternary material LiNi 1-x-y Co x Mn y O 2 (abbreviated as NCM, wherein 0<x<1, 0<y<1) Has the characteristics superior to lithium iron phosphate and lithium cobaltate, and can prepare ternary electrode materials with different properties by adjusting the proportion of nickel, cobalt and manganese. The NCM improves the structural stability of the material, improves the charge-discharge cycle stability and high-temperature stability of the material, and exerts the excellent electrochemical performance to the maximum extent.
Therefore, it is necessary to provide a new SiO 2 The method for coating the ternary cathode material further improves the electrochemical performance of the material.
Disclosure of Invention
The invention aims to provide a preparation method of a silicon dioxide coated ternary material.
Still another object of the present invention is to: provides a silicon dioxide coated ternary material product prepared by the method.
Yet another object of the present invention is: provides an application of the product.
The purpose of the invention is realized by the following scheme: a preparation method of a silicon dioxide coated ternary material is characterized by comprising the following specific steps:
(1) Nickel isopropoxide and tetrabutyl silicate were added in a 100 mmol: dissolving 1 to 3 mmol of the mixture in 70 mL absolute ethyl alcohol, carrying out ultrasonic dispersion for 20 to 30 min, and then stirring for 1 to 2 h.
(2) 10 mL deionized water was added dropwise to the suspension to form a sol.
(3) Adding lithium salt, cobalt salt and manganese salt into the sol (wherein the molar weight ratio of the lithium salt to the nickel isopropoxide to the cobalt salt to the manganese salt is 1:1-x-y: x: y), continuously stirring for 1-2 h, adding into a 100 mL reaction kettle, and reacting for 10-15 h at 160-180 ℃ to obtain SiO 2 The coated ternary precursor is washed with deionized water 3~5 times and dried in a vacuum oven at 60-80 ℃.
(4) Mixing SiO 2 Calcining the coated ternary precursor at 600 to 800 ℃ for 3 to 5 hours to obtain SiO 2 A coated ternary material.
The invention provides a preparation method of a silicon dioxide coated ternary material, which is used for improving harmful corrosion of HF to a battery material by coating SiO on the surface of a positive electrode material 2 Is an effective method. On the one hand, siO is coated 2 Isolating the anode material from the electrolyte to prevent HF from dissolving metal elements on the surface of the material; on the other hand, siO 2 Can react with a small amount of HF, reduces the corrosion of the HF to the surface of the electrode by consuming the HF, reduces the generation of impurity gas and blocks the subsequent adverse chain reaction. The invention provides a novel SiO 2 The method for coating the ternary cathode material further improves the electrochemical performance of the material.
On the basis of the scheme, the lithium salt is one or the combination of lithium hydroxide, lithium acetate or lithium formate.
The cobalt salt is one or the combination of cobalt chloride, cobalt acetate or cobalt formate.
The manganese salt is one or the combination of manganese chloride, manganese acetate or manganese formate.
The invention provides a silicon dioxide coated ternary material prepared by any one of the methods.
The invention provides an application of a silicon dioxide coated ternary material in a lithium battery positive electrode material.
The invention has the beneficial effects that:
SiO-coated film 2 Isolating the anode material from the electrolyte to prevent HF from dissolving metal elements on the surface of the material; in addition, siO 2 Can react with a small amount of HF, reduces the corrosion of the HF to the surface of the electrode by consuming the HF, reduces the generation of impurity gas and blocks the subsequent adverse chain reaction. The invention provides a novel SiO 2 The method for coating the ternary cathode material further improves the electrochemical performance of the material.
Drawings
FIG. 1 is SiO of example 1 2 Cycle life plot of the clad ternary material.
Detailed Description
The present invention is described in detail by the following specific examples, but the scope of the present invention is not limited to these examples.
Example one
A silicon dioxide coated ternary material is prepared by the following steps:
(1) Nickel isopropoxide and tetrabutyl silicate were added in a 100 mmol: dissolving 1 mmol in 70 mL absolute ethyl alcohol, performing ultrasonic dispersion for 30 min, and stirring 1h to obtain a suspension;
(2) Dropwise adding 10 mL deionized water into the suspension to form sol;
(3) Adding lithium hydroxide, cobalt chloride cobalt salt and manganese chloride manganese salt into the sol, wherein the molar weight ratio of the lithium hydroxide, the nickel isopropoxide, the cobalt chloride and the manganese chloride is 1 mmol:0.333 mmol:0.333 mmol:0.333 mmol, continuously stirring for 1h, adding into a 100 mL reaction kettle, reacting for 15h at 160 ℃ to obtain SiO 2 Washing the coated ternary precursor with deionized water for 3 times, and drying in a vacuum oven at 80 ℃;
(4) Mixing SiO 2 Calcining the coated ternary precursor at 600 ℃ for 5h to obtain SiO 2 A coated ternary material.
To obtain SiO 2 The cycle life of the coated ternary material is shown in figure 1, the first discharge specific capacity of the coated ternary material is 178.9 mAh/g, after 50 cycles, the discharge specific capacity is 174.8 mAh/g, and the capacity retention rate is 97.7%.
Example two
A silica-coated ternary material, prepared by the following steps, similar to the steps of example 1:
(1) Nickel isopropoxide and tetrabutyl silicate were added in a 100 mmol: dissolving 2mmol in 70 mL anhydrous ethanol, performing ultrasonic dispersion for 30 min, and stirring 2h to obtain suspension;
(2) Dropwise adding 10 mL deionized water into the suspension to form sol;
(3) Adding lithium acetate, cobalt acetate and manganese acetate into the sol, wherein the molar weight ratio of the lithium acetate to the nickel isopropoxide to the cobalt acetate to the manganese acetate is 1 mmol:0.5 mmol:0.3 mmol:0.2 mmol, continuously stirring 1h, adding into 100 mL reaction kettle, reacting for 12h at 170 ℃ to obtain SiO 2 Washing the coated ternary precursor with deionized water for 5 times, and drying in a vacuum oven at 80 ℃;
(4) Mixing SiO 2 Calcining the coated ternary precursor at 700 ℃ for 4h to obtain SiO 2 A coated ternary material.
EXAMPLE III
A silica-coated ternary material, prepared by the following steps, similar to the steps of example 1:
(1) Nickel isopropoxide and tetrabutyl silicate were added in a 100 mmol: dissolving 3 mmol in 70 mL anhydrous ethanol, performing ultrasonic dispersion for 20 min, and stirring 2h to obtain a suspension;
(2) Dropwise adding 10 mL deionized water into the suspension to form a sol;
(3) Adding lithium formate, cobalt formate and manganese formate into the sol, wherein the molar weight ratio of the lithium formate to the nickel isopropoxide to the cobalt formate to the manganese formate is 1 mmol:0.8 mmol:0.1 mmol:0.1 mmol, continuously stirring for 1h, adding into a 100 mL reaction kettle, reacting for 10h at 180 ℃ to obtain SiO 2 Washing the coated ternary precursor with deionized water for 5 times, and drying in a vacuum oven at 60 ℃;
(4) Mixing SiO 2 Calcining the coated ternary precursor at 800 ℃ for 3 h to obtain SiO 2 A coated ternary material.
Claims (6)
1. The preparation method of the silicon dioxide coated ternary material is characterized by comprising the following steps of:
(1) Nickel isopropoxide and tetrabutyl silicate were added in a 100 mmol: dissolving 1 to 3 mmol of the powder in 70 mL absolute ethyl alcohol, carrying out ultrasonic dispersion for 20 to 30 min, and then stirring for 1 to 2h to obtain a suspension;
(2) Dropwise adding 10 mL deionized water into the suspension to form a sol;
(3) Adding lithium salt, cobalt salt and manganese salt into the sol, wherein the molar ratio of the lithium salt to the nickel isopropoxide to the cobalt salt to the manganese salt is 1:1-x-y: x: y), continuously stirring for 1-2 h, adding into a 100 mL reaction kettle, and reacting for 10-15 h at 160-180 ℃ to obtain SiO 2 Washing the coated ternary precursor with deionized water 3~5 times, and drying in a vacuum oven at 60-80 ℃;
(4) Mixing SiO 2 Calcining the coated ternary precursor at 600-800 ℃ for 3-5 h to obtain SiO 2 A coated ternary material.
2. The method for preparing the silica-coated ternary material according to claim 1, wherein the lithium salt is one or a combination of lithium hydroxide, lithium acetate or lithium formate, or the lithium salt is replaced by atmospheric lithium hydroxide.
3. The method according to claim 1, wherein the cobalt salt is one or a combination of cobalt chloride, cobalt acetate, or cobalt formate.
4. The method according to claim 1, wherein the manganese salt is one or a combination of manganese chloride, manganese acetate, or manganese formate.
5. A silica-coated ternary material characterized by being prepared according to the process of any one of claims 1 to 4.
6. Use of the silica-coated ternary material according to claim 5 in a positive electrode material for lithium batteries.
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| CN112952066A (en) * | 2021-03-26 | 2021-06-11 | 蜂巢能源科技有限公司 | Ternary cathode material, preparation method and application thereof |
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