CN111470547A - NCM @ Al2O3Preparation method for modifying/rCO material - Google Patents
NCM @ Al2O3Preparation method for modifying/rCO material Download PDFInfo
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- CN111470547A CN111470547A CN202010278617.5A CN202010278617A CN111470547A CN 111470547 A CN111470547 A CN 111470547A CN 202010278617 A CN202010278617 A CN 202010278617A CN 111470547 A CN111470547 A CN 111470547A
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- 239000000463 material Substances 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 14
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 14
- 238000001354 calcination Methods 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- 239000002002 slurry Substances 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 6
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium chloride Substances Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 3
- 238000000151 deposition Methods 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 3
- 239000002243 precursor Substances 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- 239000000126 substance Substances 0.000 claims description 8
- 229910002804 graphite Inorganic materials 0.000 claims description 7
- 239000010439 graphite Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 5
- 230000001276 controlling effect Effects 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 230000007246 mechanism Effects 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-UHFFFAOYSA-N 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 238000000354 decomposition reaction Methods 0.000 claims description 2
- 125000000524 functional group Chemical group 0.000 claims description 2
- 238000003837 high-temperature calcination Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000001338 self-assembly Methods 0.000 claims description 2
- 238000000576 coating method Methods 0.000 abstract description 21
- 239000011248 coating agent Substances 0.000 abstract description 19
- 230000008569 process Effects 0.000 abstract description 4
- 230000004048 modification Effects 0.000 abstract description 3
- 238000012986 modification Methods 0.000 abstract description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 239000011247 coating layer Substances 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000009795 derivation Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/14—Aluminium oxide or hydroxide from alkali metal aluminates
- C01F7/141—Aluminium oxide or hydroxide from alkali metal aluminates from aqueous aluminate solutions by neutralisation with an acidic agent
- C01F7/142—Aluminium oxide or hydroxide from alkali metal aluminates from aqueous aluminate solutions by neutralisation with an acidic agent with carbon dioxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
Abstract
The invention relates to the technical field of ternary material coating modification, in particular to NCM @ Al2O3The preparation method for modifying the/rGO material comprises the following steps: step 1: dissolving graphene oxide slurry in deionized water, ultrasonically stirring for 30min, and then adding AlCl3Stirring for 30min, adding dropwise ammonia water, and adjusting pH to Al (OH)3Depositing the precursor in a form on an rGO sheet layer, then adding an NCM ternary material, and stirring to obtain a mixture; step 2: transferring the mixture into a high-pressure reaction kettle, and leading Al (OH) to react by a hydrothermal reaction3the/rGO is uniformly coated on the surface of the NCM material; and step 3: washing the prepared hydrothermal product by using deionized water, and then drying in vacuum; and 4, step 4: placing into a tube furnace, performing heat treatment in Ar gas state, and calcining at high temperature to obtain Al (OH)3/rGDecomposition of O into Al2O3the/rGO is coated on the surface of the ternary material. The method has simple process and mild conditions, and can greatly improve the electrochemical performance of the ternary coating material.
Description
Technical Field
The invention relates to the technical field of ternary material coating modification, in particular to NCM @ Al2O3A preparation method for modifying rGO material.
Background
The common ternary material coating method comprises carbon coating, double-layer coating (carbon-carbon and carbon-silicon) metal oxide composite coating and the like, and the coatings play a role in reducing side reactions and effectively improve the electrochemical cycle performance of the coating; however, the uniformity of coating and the thickness control of the coating layer are still difficult, and meanwhile, the compactness of the coating material also influences the gram capacity of the ternary material; at present, the coating solves the problems of uniformity and coating thickness by a sol-gel method, but the problem of compactness of the coating material is still difficult to solve.
Disclosure of Invention
The invention aims to provide NCM @ Al2O3The preparation method of the modification of the/rCO material has the advantages of simple process and mild conditions, can realize the uniform coating of the ternary material to a great extent, and simultaneously improves the compactness of the coating material, so that the coating material has the advantages of high gram volume and strong electric conductivity, and finally improves the electrochemical performance of the ternary coating material.
The technical scheme of the invention is as follows:
NCM @ Al2O3The preparation method for modifying the/rGO material comprises the following steps:
step 1: dissolving graphene oxide slurry prepared from natural crystalline flake graphite in 500ml of deionized water, ultrasonically stirring for 30min, and then adding AlCl3Stirring for 30min, adding dropwise ammonia water, and adjusting pH to Al (OH)3Depositing the precursor in a form on an rGO (reduced graphene oxide) sheet layer, then adding an NCM (ternary nickel cobalt manganese) material, stirring for 20min, and uniformly mixing to obtain a mixture;
step 2: transferring the mixture prepared in the step 1 into a high-pressure reaction kettle, reducing GO through a hydrothermal reaction, and enabling Al (OH) to be subjected to self-assembly of rGO in the process3/rGO is homogeneousCoating on the surface of the NCM material;
and step 3: washing the hydrothermal product prepared in the step 2 with deionized water, then drying in vacuum for a certain time, regulating and controlling the three-dimensional structure of the graphene material by using a capillary evaporation method, and improving the density of the material by using a mechanism of driving the flexible sheet to be densified by a solvent;
and 4, step 4: putting the vacuum dried substance obtained in the step 3 into a tubular furnace, carrying out heat treatment in an Ar gas state, further removing oxygen-containing functional groups of the rGO, improving the conductivity of the rGO, and then carrying out high-temperature calcination to enable Al (OH)3Decomposition of/rGO to Al2O3the/rGO is coated on the surface of the ternary material.
Preferably, the mesh number of the natural crystalline flake graphite in the step 1 is preferably 100 to 5000 meshes, and most preferably 325 to 2000 meshes.
Preferably, AlCl is used in step 13The mass ratio of the NCM to the GO is 1: 7.5-1: 19, and the mass ratio of the NCM to the GO is 2.4: 1-0.96: 1.
Preferably, the pH value of the mixture in the step 1 is 9-11.
Preferably, in the high-pressure reaction kettle in the step 2, the temperature is most preferably 160-200 ℃, and the reaction time is 9-18 h.
Preferably, the temperature of the vacuum drying in the step 3 is most preferably 20-40 ℃, and the time is 12-24 h.
Preferably, the solvent in step 3 is water, and the amount is 500 ml.
Preferably, the heat treatment temperature in the step 4 is preferably 140-160 ℃, the heat treatment time is 1-2 h, the calcination temperature is preferably 800-1000 ℃, and the calcination time is 2-4 h.
The invention has the beneficial effects that:
1. the coating layer can effectively inhibit the structural change of the ternary high nickel material in the charging and discharging process, reduce the direct contact between the ternary high nickel material and electrolyte and the dissolution of surface transition metal in the electrolyte, reduce the occurrence of side reaction and effectively improve the electrochemical cycle performance of the ternary high nickel material.
2. The controllable and uniform coating of the coating layer can be realized by controlling the quality and the temperature of the coating material by adopting a liquid phase sol-gel method.
3. The rGO structure is regulated and controlled by adopting a capillary evaporation method, and the compactness of the material is improved by a mechanism of driving the densification of the flexible sheet layer by a solvent, so that the electrochemical properties such as gram capacity and the like of the coating material are improved.
4. Simple process, mild condition and safe operation.
Drawings
FIG. 1 is sample NCM @ Al (OH)3SEM image before/rGO calcination.
FIG. 2 is sample NCM @ Al (OH)3SEM image after calcination of/rGO.
Detailed Description
The following describes the embodiments of the present invention in detail with reference to fig. 1 and 2.
Example 1:
NCM @ Al2O3The preparation method of the modified/rGO material comprises the following steps:
1. preparing 325-2000 mesh natural crystalline flake graphite into graphene oxide slurry, putting 10ml of the slurry into a beaker, adding deionized water to prepare 500ml of mixed solution, and ultrasonically stirring for 30 min.
2. Then 2.67g of AlCl was added3Adding into the mixed solution, stirring for 20min to dissolve completely, adding dropwise ammonia water while stirring, adjusting pH to 9, adding 48g of NCM ternary material, stirring for 20min to mix well;
3. transferring the uniformly mixed substances into a high-pressure reaction kettle, and reacting for 24 hours at 160 ℃.
4. After the reaction is finished, the product is washed for three times and then dried in a vacuum drying oven for 24 hours at the temperature of 20 ℃.
5. Putting the dried substance into a tube furnace, carrying out heat treatment for 2h at 140 ℃ in Ar atmosphere, and calcining for 4h at 800 ℃ to obtain the final product NCM @ Al2O3/rGO。
Sample NCM @ Al (OH)3SEM images before/rGO calcination are shown in FIG. 1.
Sample NCM @ Al (OH)3SEM images of/rGO after calcination are shown in FIG. 2.
Example 2:
NCM @ Al2O3The preparation method of the modified/rGO material comprises the following steps:
1. preparing 325-2000 mesh natural crystalline flake graphite into graphene oxide slurry, putting 10ml of the slurry into a beaker, adding deionized water to prepare 500ml of mixed solution, and ultrasonically stirring for 30 min.
2. 6.76g of AlCl was added3Adding into the mixed solution, stirring for 20min to dissolve completely, adding dropwise ammonia water while stirring, adjusting pH to 11, adding 19.2g of NCM ternary raw material, and stirring for 20min to mix well;
3. transferring the uniformly mixed substances into a high-pressure reaction kettle, and reacting for 12 hours at 200 ℃.
4. After the reaction, the product was washed three times and dried in a vacuum oven at 30 ℃ for 12 hours.
5. Putting the dried substance into a tube furnace, carrying out heat treatment for 1h at 160 ℃ in Ar atmosphere, and calcining for 2h at 1000 ℃ to obtain the final product NCM @ Al2O3/rGO。
Example 3:
NCM @ Al2O3The preparation method of the modified/rGO material comprises the following steps:
1. preparing 325-2000 mesh natural crystalline flake graphite into graphene oxide slurry, putting 10ml of the slurry into a beaker, adding deionized water to prepare 500ml of mixed solution, and ultrasonically stirring for 30 min.
2. 5.30g of AlCl was added3Stirring for 20min to dissolve completely, adding dropwise ammonia water while stirring, adjusting pH to 10, collecting 25g NCM ternary material, and stirring for 20min to mix well;
3. transferring the uniformly mixed substances into a high-pressure reaction kettle, and reacting for 16h at 180 ℃.
4. After the reaction, the product was washed three times and dried in a vacuum oven at 25 ℃ for 18 h.
5. Placing the dried substance into a tube furnace, performing heat treatment at 150 deg.C for 1.5h in Ar gas atmosphere, and calcining at 900 deg.C for 3h to obtainTo the final product NCM @ Al2O3/rGO。
The foregoing is merely a preferred embodiment of the invention and all such equivalent alterations and permutations and derivations thereof are intended to be included within the scope of the invention.
Claims (8)
1. NCM @ Al2O3The preparation method for modifying the/rGO material is characterized by comprising the following steps:
step 1: dissolving graphene oxide slurry prepared from natural crystalline flake graphite in 500ml of deionized water, ultrasonically stirring for 30min, and then adding AlCl3Stirring for 30min, adding dropwise ammonia water, and adjusting pH to Al (OH)3Depositing the precursor in a form on an rGO (reduced graphene oxide) sheet layer, then adding an NCM (ternary nickel cobalt manganese) material, stirring for 20min, and uniformly mixing to obtain a mixture;
step 2: transferring the mixture prepared in the step 1 into a high-pressure reaction kettle, reducing GO through a hydrothermal reaction, and enabling Al (OH) to be subjected to self-assembly of rGO in the process3the/rGO is uniformly coated on the surface of the NCM material;
and step 3: washing the hydrothermal product prepared in the step 2 with deionized water, then drying in vacuum for a certain time, regulating and controlling the three-dimensional structure of the graphene material by using a capillary evaporation method, and improving the density of the material by using a mechanism of driving the flexible sheet to be densified by a solvent;
and 4, step 4: putting the vacuum dried substance obtained in the step 3 into a tubular furnace, carrying out heat treatment in an Ar gas state, further removing oxygen-containing functional groups of the rGO, improving the conductivity of the rGO, and then carrying out high-temperature calcination to enable Al (OH)3Decomposition of/rGO to Al2O3the/rGO is coated on the surface of the ternary material.
2. The NCM @ Al of claim 12O3The preparation method for modifying the/rGO material is characterized by comprising the following steps: the mesh number of the natural crystalline flake graphite in the step 1 is preferably 100-5000 meshes, and most preferably 325-2000 meshes.
3. According to the rightNCM @ Al as claimed in claim 12O3The preparation method for modifying the/rGO material is characterized by comprising the following steps: AlCl described in step 13The mass ratio of the NCM to the GO is 1: 7.5-1: 19, and the mass ratio of the NCM to the GO is 2.4: 1-0.96: 1.
4. The NCM @ Al of claim 12O3The preparation method for modifying the/rGO material is characterized by comprising the following steps: the pH value range of the mixture in the step 1 is 9-11.
5. The NCM @ Al of claim 12O3The preparation method for modifying the/rGO material is characterized by comprising the following steps: in the high-pressure reaction kettle in the step 2, the temperature is preferably 160-200 ℃, and the reaction time is 9-18 h.
6. The NCM @ Al of claim 12O3The preparation method for modifying the/rGO material is characterized by comprising the following steps: the temperature of the vacuum drying in the step 3 is most preferably 20-40 ℃, and the time is 12-24 h.
7. The NCM @ Al of claim 12O3The preparation method for modifying the/rGO material is characterized by comprising the following steps: the solvent in the step 3 is water, and the using amount is 500 ml.
8. The NCM @ Al of claim 12O3The preparation method for modifying the/rGO material is characterized by comprising the following steps: the heat treatment temperature in the step 4 is preferably 140-160 ℃, the heat treatment time is 1-2 h, the calcination temperature is preferably 800-1000 ℃, and the calcination time is 2-4 h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112151742A (en) * | 2020-09-25 | 2020-12-29 | 福建师范大学 | Preparation method of ternary cathode material modified by metal oxide and graphene and used for improving performance of full battery |
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