CN105024078A - Preparation method for Ni-Co-Al-Mg oxide cladded carbon nanotubes for lithium ion battery - Google Patents
Preparation method for Ni-Co-Al-Mg oxide cladded carbon nanotubes for lithium ion battery Download PDFInfo
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Abstract
The invention discloses a preparation method for Ni-Co-Al-Mg oxide cladded carbon nanotubes for a lithium ion battery. The preparation method comprises the following steps of: dissolving a nickel salt, a cobalt salt, a magnesium salt and an aluminum salt into water, and adding a slow controlled agent to prepare a mixed solution A; simultaneously adding the mixed solution A and a precipitating agent into a container for co-precipitation; carrying out purification, heat stabilizing and sub-high temperature treatment on the sediment to prepare the Ni-Co-Al-Mg oxide; mixing the Ni-Co-Al-Mg oxide and 2 wt% poly diallyldimethylammonium chloride (PDDA) aqueous solution, and subjecting the solution to ultrasound treatment; mixing the solution with a prepared carbon nano tube solution; and subjecting the solution to ultrasound treatment, and filtering and drying the solution to obtain the Ni-Co-Al-Mg oxide cladded carbon nanotubes for the lithium ion battery. The material has the advantages of high utilization rate, stable performance, excellent cycle performance and rate capability, no toxin and no harm to environment, and moreover, the preparation method is simple, is short in reaction time, low in cost and mild in condition, and is easy to control.
Description
Technical field:
The present invention relates to field of lithium ion battery, be specifically related to the preparation method of a kind of lithium ion battery carbon nano-tube coated nickel cobalt magnalium oxide.
Background technology:
Along with the continuous deterioration of earth atmosphere environment, people more and more pay attention to the exploitation of the New Technologies of clean energy resource and energy storage material.Lithium-ion-power cell has high-energy-density, high security, the superperformance such as renewable because of it, arouses great concern.The development of special auto industry in global general population is popularized, in order to avoid the tail gas of gasoline car generation is on the impact of air, for the wide prospect that the development of electric automobile provides, thus be the power lithium-ion battery positive electrode of its property used and presoma thereof, great demand will be brought.
Current driving force lithium ion battery presoma mainly contains cobaltosic oxide, manganese sesquioxide managnic oxide, di iron, cobalt oxide nickel, hydroxyl nickel cobalt manganese, carbonyl cobalt magnesium manganese etc., its process route prepared, according to preparation form be divided into wet method, dry method or the two go here and there and have concurrently.Chemical precipitation method is had according to the chemism of preparation, electrochemical process, oxidation-reduction method, metathesis reaction and this several mechanism comprehensive etc., the agitating mode of main reaction process has gas sparging method, advance paddling process, external force damped method etc. one or several have concurrently, the auxiliary agent of preparation process has amino-compound, one or more simultaneously dual-purposes such as ammonium salt, show according to related data, material lattice prepared by these technology is unstable, chemical property is poor, harmful material is usually discharged in preparation process, and the positive electrode electric conductivity difference of preparation, ionic diffusion coefficient is low, cycle performance is poor, useful life is short.
Summary of the invention:
The object of this invention is to provide the preparation method of a kind of lithium ion battery carbon nano-tube coated nickel cobalt magnalium oxide, its lithium ion battery carbon nano-tube coated nickel cobalt magnalium oxidation material utilance prepared is high, stable performance, cycle performance and high rate performance excellence, nontoxic, environmental sound, and its preparation method is simple, reaction time is short, mild condition, be easy to control, cost is low.
For achieving the above object, the present invention adopts following beneficial effect:
A preparation method for lithium ion battery carbon nano-tube coated nickel cobalt magnalium oxide, comprises the following steps:
(1) nickel salt, cobalt salt, magnesium salts, aluminium salt are dissolved in water, add slow control agent, under the power of 500-800W, ultrasonic 1-2h, obtained mixed solution A;
(2) by mixed solution A obtained for step (1) and precipitation reagent respectively with 0.5-8 l/h, the speed of 0.01-6 l/h joins in reaction vessel and reacts, and guarantee that the material in reaction vessel is in radial and axial motion, the water of sediment 60-80 DEG C that obtains after reaction repeatedly washs, and obtains class spherical nickel-cobalt aluminum-magnesium hydroxide matrix;
(3) class spherical nickel-cobalt aluminum-magnesium hydroxide matrix step (2) obtained is after heat setting 2-5h, and sub-high-temperature process 12-24h, obtains nickel cobalt magnalium oxide;
(4) prepare the aqueous solution of the PDDA of 2wt%, and mix with the nickel cobalt magnalium that step (3) obtains, under the state of 2000-5000 rev/min, stir 2-5h, filter, dry, obtain the nickel cobalt magnalium oxide that PDDA modifies;
(5) carbon nano-tube is mixed with water, under the power of 400-600W, ultrasonic 20-50min, obtain the aqueous dispersions of carbon nano-tube, add the nickel cobalt magnalium oxide of the PDDA modification that step (4) obtains again, continue ultrasonic 1-3h, filter, vacuumize, obtains lithium ion battery carbon nano-tube coated nickel cobalt magnalium oxide.
Preferred as technique scheme, in step (1), described nickel salt is nickel chloride, nickel nitrate, the one or any two kinds of mixing of nickelous sulfate, described cobalt salt is cobalt chloride, cobalt nitrate, the one or any two kinds of mixing of cobaltous sulfate, described aluminium salt is manganese chloride, manganese nitrate, the one or any two kinds of mixing of manganese sulfate, and described magnesium salts is magnesium chloride, the one or any two kinds of mixing of magnesium nitrate.
Preferred as technique scheme, in step (1), described slow control agent is one or both mixing in citric acid, oxalic acid.
Preferred as technique scheme, in step (2), the speed that adds of (1) mixed solution A and precipitation reagent is respectively 2.5 ls/h, 1.25 ls/h.
Preferred as technique scheme, in step (2), the pH of described reaction is 9-14, and temperature is 50-85 DEG C.
Preferred as technique scheme, described precipitation reagent is one or both mixing in potassium hydroxide, NaOH.
Preferred as technique scheme, in step (3), the condition of described heat setting is 80-130 DEG C, pressure 0-0.01Mpa, the air atmosphere of oxygen volumn concentration 14-20%; Described sub-high-temperature process condition is 600-800 DEG C, pressure 0-0.1Mpa, the air atmosphere of oxygen volumn concentration 14-20%.
Preferred as technique scheme, in step (4), the aqueous solution of the PDDA of 2wt% and the mass ratio of nickel cobalt magnalium oxide are 50-100:1.
Preferred as technique scheme, in step (5), when carbon nano-tube mixes with water, both mass ratioes are 1:100.
Preferred as technique scheme, in step (5), the mass ratio of the nickel cobalt magnalium oxide that the aqueous dispersions of carbon nano-tube and PDDA modify is 100-200:1.
The present invention has following beneficial effect:
This preparation method is simple, preparation process does not produce environmentally harmful containing ammonia nitrogen substances, the nickel cobalt magnalium oxide lattice prepared, structure cell are regular, spherical particle is large and solid, the migration such as other atoms, ion, electronics evenly, thus improves the chemical property of corresponding product, the stability of structure; The nickel cobalt magnalium oxide of PDDA modified, mix with the aqueous dispersions of carbon nano-tube, can at the oxide surface adsorbing carbon nanotubes of modified, and adsorption layer is even, substantially increase the conductance of nickel cobalt magnalium oxide surface, this positive electrode cycle performance and high rate performance also improve greatly.
Embodiment:
For a better understanding of the present invention, below by embodiment, the present invention is further described, and embodiment, only for explaining the present invention, can not form any restriction to the present invention.
Embodiment 1
(1) nickel salt, cobalt salt, magnesium salts, aluminium salt are dissolved in water, add slow control agent, under the power of 500W, ultrasonic 1h, obtained mixed solution A;
(2) mixed solution A step (1) obtained and precipitation reagent join in reaction vessel with the speed of 0.5 l/h, 0.01 l/h respectively and react, and guarantee that the material in reaction vessel is in radial and axial motion, reaction pH is 9, temperature is 50 DEG C, the water of sediment 60-80 DEG C that obtains after reaction repeatedly washs, and obtains class spherical nickel-cobalt aluminum-magnesium hydroxide matrix;
(3) class spherical nickel-cobalt aluminum-magnesium hydroxide matrix step (2) obtained is at 80 DEG C, pressure 0-0.01Mpa, under the air atmosphere of oxygen volumn concentration 14-20% after heat setting 2h, at 600 DEG C, pressure 0-0.1Mpa, sub-high-temperature process 12h under the air atmosphere of oxygen volumn concentration 14-20%, obtains nickel cobalt magnalium oxide;
(4) prepare the aqueous solution of the PDDA of 2wt%, and mix with the nickel cobalt magnalium that step (3) obtains, under the state of 2000 revs/min, stir 2h, filter, dry, obtain the nickel cobalt magnalium oxide that PDDA modifies;
(5) carbon nano-tube is mixed with water, under the power of 400W, ultrasonic 20min, obtain the aqueous dispersions of carbon nano-tube, add the nickel cobalt magnalium oxide of the PDDA modification that step (4) obtains again, continue ultrasonic 1h, filter, vacuumize, obtains lithium ion battery carbon nano-tube coated nickel cobalt magnalium oxide.
Embodiment 2
(1) nickel salt, cobalt salt, magnesium salts, aluminium salt are dissolved in water, add slow control agent, under the power of 800W, ultrasonic 2h, obtained mixed solution A;
(2) mixed solution A step (1) obtained and precipitation reagent join in reaction vessel with the speed of 8 ls/h, 6 ls/h respectively and react, and guarantee that the material in reaction vessel is in radial and axial motion, reaction pH is 14, temperature is 85 DEG C, the water of sediment 60-80 DEG C that obtains after reaction repeatedly washs, and obtains class spherical nickel-cobalt aluminum-magnesium hydroxide matrix;
(3) class spherical nickel-cobalt aluminum-magnesium hydroxide matrix step (2) obtained is at 130 DEG C, pressure 0-0.01Mpa, under the air atmosphere of oxygen volumn concentration 14-20% after heat setting 5h, at 800 DEG C, pressure 0-0.1Mpa, sub-high-temperature process 24h under the air atmosphere of oxygen volumn concentration 14-20%, obtains nickel cobalt magnalium oxide;
(4) prepare the aqueous solution of the PDDA of 2wt%, and mix with the nickel cobalt magnalium that step (3) obtains, under the state of 5000 revs/min, stir 5h, filter, dry, obtain the nickel cobalt magnalium oxide that PDDA modifies;
(5) carbon nano-tube is mixed with water, under the power of 600W, ultrasonic 50min, obtain the aqueous dispersions of carbon nano-tube, add the nickel cobalt magnalium oxide of the PDDA modification that step (4) obtains again, continue ultrasonic 3h, filter, vacuumize, obtains lithium ion battery carbon nano-tube coated nickel cobalt magnalium oxide.
Embodiment 3
(1) nickel salt, cobalt salt, magnesium salts, aluminium salt are dissolved in water, add slow control agent, under the power of 600W, ultrasonic 1.2h, obtained mixed solution A;
(2) mixed solution A step (1) obtained and precipitation reagent join in reaction vessel with the speed of 2.5 ls/h, 1.5 ls/h respectively and react, and guarantee that the material in reaction vessel is in radial and axial motion, reaction pH is 10, temperature is 60 DEG C, the water of sediment 60-80 DEG C that obtains after reaction repeatedly washs, and obtains class spherical nickel-cobalt aluminum-magnesium hydroxide matrix;
(3) class spherical nickel-cobalt aluminum-magnesium hydroxide matrix step (2) obtained is at 90 DEG C, pressure 0-0.01Mpa, under the air atmosphere of oxygen volumn concentration 14-20% after heat setting 2.5h, at 650 DEG C, pressure 0-0.1Mpa, sub-high-temperature process 14h under the air atmosphere of oxygen volumn concentration 14-20%, obtains nickel cobalt magnalium oxide;
(4) prepare the aqueous solution of the PDDA of 2wt%, and mix with the nickel cobalt magnalium that step (3) obtains, under the state of 3000 revs/min, stir 2.5h, filter, dry, obtain the nickel cobalt magnalium oxide that PDDA modifies;
(5) carbon nano-tube is mixed with water, under the power of 450W, ultrasonic 25min, obtain the aqueous dispersions of carbon nano-tube, add the nickel cobalt magnalium oxide of the PDDA modification that step (4) obtains again, continue ultrasonic 1.5h, filter, vacuumize, obtains lithium ion battery carbon nano-tube coated nickel cobalt magnalium oxide.
Embodiment 4
(1) nickel salt, cobalt salt, magnesium salts, aluminium salt are dissolved in water, add slow control agent, under the power of 650W, ultrasonic 1.4h, obtained mixed solution A;
(2) mixed solution A step (1) obtained and precipitation reagent join in reaction vessel with the speed of 3.5 ls/h, 2.5 ls/h respectively and react, and guarantee that the material in reaction vessel is in radial and axial motion, reaction pH is 11, temperature is 65 DEG C, the water of sediment 60-80 DEG C that obtains after reaction repeatedly washs, and obtains class spherical nickel-cobalt aluminum-magnesium hydroxide matrix;
(3) class spherical nickel-cobalt aluminum-magnesium hydroxide matrix step (2) obtained is at 100 DEG C, pressure 0-0.01Mpa, under the air atmosphere of oxygen volumn concentration 14-20% after heat setting 3h, at 700 DEG C, pressure 0-0.1Mpa, sub-high-temperature process 18h under the air atmosphere of oxygen volumn concentration 14-20%, obtains nickel cobalt magnalium oxide;
(4) prepare the aqueous solution of the PDDA of 2wt%, and mix with the nickel cobalt magnalium that step (3) obtains, under the state of 3500 revs/min, stir 3h, filter, dry, obtain the nickel cobalt magnalium oxide that PDDA modifies;
(5) carbon nano-tube is mixed with water, under the power of 500W, ultrasonic 30min, obtain the aqueous dispersions of carbon nano-tube, add the nickel cobalt magnalium oxide of the PDDA modification that step (4) obtains again, continue ultrasonic 2h, filter, vacuumize, obtains lithium ion battery carbon nano-tube coated nickel cobalt magnalium oxide.
Embodiment 5
(1) nickel salt, cobalt salt, magnesium salts, aluminium salt are dissolved in water, add slow control agent, under the power of 700W, ultrasonic 1.6h, obtained mixed solution A;
(2) mixed solution A step (1) obtained and precipitation reagent join in reaction vessel with the speed of 5.5 ls/h, 3.5 ls/h respectively and react, and guarantee that the material in reaction vessel is in radial and axial motion, reaction pH is 12, temperature is 75 DEG C, the water of sediment 60-80 DEG C that obtains after reaction repeatedly washs, and obtains class spherical nickel-cobalt aluminum-magnesium hydroxide matrix;
(3) class spherical nickel-cobalt aluminum-magnesium hydroxide matrix step (2) obtained is at 110 DEG C, pressure 0-0.01Mpa, under the air atmosphere of oxygen volumn concentration 14-20% after heat setting 3.5h, at 750 DEG C, pressure 0-0.1Mpa, sub-high-temperature process 20h under the air atmosphere of oxygen volumn concentration 14-20%, obtains nickel cobalt magnalium oxide;
(4) prepare the aqueous solution of the PDDA of 2wt%, and mix with the nickel cobalt magnalium that step (3) obtains, under the state of 4000 revs/min, stir 3.5h, filter, dry, obtain the nickel cobalt magnalium oxide that PDDA modifies;
(5) carbon nano-tube is mixed with water, under the power of 550W, ultrasonic 35min, obtain the aqueous dispersions of carbon nano-tube, add the nickel cobalt magnalium oxide of the PDDA modification that step (4) obtains again, continue ultrasonic 2.5h, filter, vacuumize, obtains lithium ion battery carbon nano-tube coated nickel cobalt magnalium oxide.
Embodiment 6
(1) nickel salt, cobalt salt, magnesium salts, aluminium salt are dissolved in water, add slow control agent, under the power of 800W, ultrasonic 1.8h, obtained mixed solution A;
(2) mixed solution A step (1) obtained and precipitation reagent join in reaction vessel with the speed of 7.5 ls/h, 5.5 ls/h respectively and react, and guarantee that the material in reaction vessel is in radial and axial motion, reaction pH is 13, temperature is 80 DEG C, the water of sediment 60-80 DEG C that obtains after reaction repeatedly washs, and obtains class spherical nickel-cobalt aluminum-magnesium hydroxide matrix;
(3) class spherical nickel-cobalt aluminum-magnesium hydroxide matrix step (2) obtained is at 120 DEG C, pressure 0-0.01Mpa, under the air atmosphere of oxygen volumn concentration 14-20% after heat setting 4.5h, at 800 DEG C, pressure 0-0.1Mpa, sub-high-temperature process 22h under the air atmosphere of oxygen volumn concentration 14-20%, obtains nickel cobalt magnalium oxide;
(4) prepare the aqueous solution of the PDDA of 2wt%, and mix with the nickel cobalt magnalium that step (3) obtains, under the state of 4500 revs/min, stir 4.5h, filter, dry, obtain the nickel cobalt magnalium oxide that PDDA modifies;
(5) carbon nano-tube is mixed with water, under the power of 580W, ultrasonic 45min, obtain the aqueous dispersions of carbon nano-tube, add the nickel cobalt magnalium oxide of the PDDA modification that step (4) obtains again, continue ultrasonic 3h, filter, vacuumize, obtains lithium ion battery carbon nano-tube coated nickel cobalt magnalium oxide.
Claims (10)
1. a preparation method for lithium ion battery carbon nano-tube coated nickel cobalt magnalium oxide, is characterized in that, comprise the following steps:
(1) nickel salt, cobalt salt, magnesium salts, aluminium salt are dissolved in water, add slow control agent, under the power of 500-800W, ultrasonic 1-2h, obtained mixed solution A;
(2) by mixed solution A obtained for step (1) and precipitation reagent respectively with 0.5-8 l/h, the speed of 0.01-6 l/h joins in reaction vessel and reacts, and guarantee that the material in reaction vessel is in radial and axial motion, the water of sediment 60-80 DEG C that obtains after reaction repeatedly washs, and obtains class spherical nickel-cobalt aluminum-magnesium hydroxide matrix;
(3) class spherical nickel-cobalt aluminum-magnesium hydroxide matrix step (2) obtained is after heat setting 2-5h, and sub-high-temperature process 12-24h, obtains nickel cobalt magnalium oxide;
(4) prepare the aqueous solution of the PDDA of 2wt%, and mix with the nickel cobalt magnalium that step (3) obtains, under the state of 2000-5000 rev/min, stir 2-5h, filter, dry, obtain the nickel cobalt magnalium oxide that PDDA modifies;
(5) carbon nano-tube is mixed with water, under the power of 400-600W, ultrasonic 20-50min, obtain the aqueous dispersions of carbon nano-tube, add the nickel cobalt magnalium oxide of the PDDA modification that step (4) obtains again, continue ultrasonic 1-3h, filter, vacuumize, obtains lithium ion battery carbon nano-tube coated nickel cobalt magnalium oxide.
2. the preparation method of a kind of lithium ion battery carbon nano-tube as claimed in claim 1 coated nickel cobalt magnalium oxide, it is characterized in that: in step (1), described nickel salt is nickel chloride, nickel nitrate, the one or any two kinds of mixing of nickelous sulfate, described cobalt salt is cobalt chloride, cobalt nitrate, the one or any two kinds of mixing of cobaltous sulfate, described aluminium salt is manganese chloride, manganese nitrate, the one or any two kinds of mixing of manganese sulfate, and described magnesium salts is magnesium chloride, the one or any two kinds of mixing of magnesium nitrate.
3. the preparation method of a kind of lithium ion battery carbon nano-tube as claimed in claim 1 coated nickel cobalt magnalium oxide, is characterized in that: in step (1), and described slow control agent is one or both mixing in citric acid, oxalic acid.
4. the preparation method of a kind of lithium ion battery carbon nano-tube as claimed in claim 1 coated nickel cobalt magnalium oxide, it is characterized in that: in step (2), the speed that adds of (1) mixed solution A and precipitation reagent is respectively 2.5 ls/h, 1.25 ls/h.
5. the preparation method of a kind of lithium ion battery carbon nano-tube as claimed in claim 1 coated nickel cobalt magnalium oxide, is characterized in that: in step (2), and the pH of described reaction is 9-14, and temperature is 50-85 DEG C.
6. the preparation method of a kind of lithium ion battery carbon nano-tube as claimed in claim 1 coated nickel cobalt magnalium oxide, is characterized in that: described precipitation reagent is one or both mixing in potassium hydroxide, NaOH.
7. the preparation method of a kind of lithium ion battery carbon nano-tube as claimed in claim 1 coated nickel cobalt magnalium oxide, it is characterized in that: in step (3), the condition of described heat setting is 80-130 DEG C, pressure 0-0.01Mpa, the air atmosphere of oxygen volumn concentration 14-20%; Described sub-high-temperature process condition is 600-800 DEG C, pressure 0-0.1Mpa, the air atmosphere of oxygen volumn concentration 14-20%.
8. the preparation method of a kind of lithium ion battery carbon nano-tube as claimed in claim 1 coated nickel cobalt magnalium oxide, is characterized in that: in step (4), and the aqueous solution of the PDDA of 2wt% and the mass ratio of nickel cobalt magnalium oxide are 50-100:1.
9. the preparation method of a kind of lithium ion battery carbon nano-tube as claimed in claim 1 coated nickel cobalt magnalium oxide, it is characterized in that: in step (5), when carbon nano-tube mixes with water, both mass ratioes are 1:100.
10. the preparation method of a kind of lithium ion battery carbon nano-tube as claimed in claim 1 coated nickel cobalt magnalium oxide, it is characterized in that: in step (5), the mass ratio of the nickel cobalt magnalium oxide that the aqueous dispersions of carbon nano-tube and PDDA modify is 100-200:1.
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| CN106450279A (en) * | 2016-10-28 | 2017-02-22 | 武汉理工大学 | Preparation method of graphene coated nickel cobalt manganese lithium ion battery cathode material |
| CN114656828A (en) * | 2022-03-09 | 2022-06-24 | 青岛爱尔家佳新材料股份有限公司 | Flame-retardant polyurea for new energy battery box and preparation method thereof |
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| CN101863519A (en) * | 2010-06-13 | 2010-10-20 | 浙江亿利泰钴镍材料有限公司 | Preparation method for nickel-cobalt-manganese ternary hydroxide for lithium battery and product |
| CN102456867A (en) * | 2010-10-19 | 2012-05-16 | 宝时得集团有限公司 | Electrode material, positive electrode, battery with positive electrode, and preparation method for electrode material |
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| CN106450279B (en) * | 2016-10-28 | 2018-12-28 | 武汉理工大学 | A kind of preparation method of graphene coated nickel cobalt manganese anode material for lithium-ion batteries |
| CN114656828A (en) * | 2022-03-09 | 2022-06-24 | 青岛爱尔家佳新材料股份有限公司 | Flame-retardant polyurea for new energy battery box and preparation method thereof |
| CN114656828B (en) * | 2022-03-09 | 2022-11-22 | 青岛爱尔家佳新材料股份有限公司 | Flame-retardant polyurea for new energy battery box and preparation method thereof |
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