CN103227314A - Preparation method of ternary cathode material - Google Patents

Preparation method of ternary cathode material Download PDF

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CN103227314A
CN103227314A CN2013101320229A CN201310132022A CN103227314A CN 103227314 A CN103227314 A CN 103227314A CN 2013101320229 A CN2013101320229 A CN 2013101320229A CN 201310132022 A CN201310132022 A CN 201310132022A CN 103227314 A CN103227314 A CN 103227314A
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cathode material
salt
preparation
cobalt
tertiary cathode
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CN103227314B (en
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李春雷
李永立
夏锋山
李东仁
马彦
李世友
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Jiayuguan Dayou Jianeng Fine Carbon Technology Co ltd
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JIAYUGUAN DAYOU JIANENG CHEMICAL CO Ltd
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Abstract

The invention discloses a preparation method of a ternary cathode material. The method includes: dissolving a lithium salt, a nickel salt, a manganese salt and a cobalt salt in an alcohol compound solvent according to certain mole ratio, then stirring them and introducing air or oxygen continuously, adding concentrated ammonia water or ammonia, raising the temperature to 80-120DEG C, and conducting roasting in a high temperature furnace at 800-950DEG C for 6-24h, thus obtaining submicron scale particles of the ternary cathode material LiNi1/3Mn1/3Co1/3O2, LiNi0.4Mn0.4Co0.2O2, LiNi0.5Mn0.3Co0.2O2 and LiNi0.7Mn0.15Co0.15O2. For the preparation method, as manganese ions and cobalt ions are subjected to pre-oxidation in a precursor preparation process, the oxidation states of manganese ions and cobalt ions in the precursor are improved, low temperature oxidation at 350-450DEG C is not needed, and the product preparation time is greatly shortened. The method does not introduce hetero-metal ions in the preparation process, and the preparation process is simple and fast. The prepared product particles are uniform in size, which ranges from 200 to 300nm, and the particles are uniformly dispersed.

Description

A kind of preparation method of tertiary cathode material
Technical field
The invention belongs to electrochemical field, relate in particular to a kind of preparation method of submicron order nickel-cobalt-manganese ternary positive electrode.
Background technology
Tertiary cathode material is a kind of composite material with cobalt, nickel, manganese trielement synergistic effect: a Co energy stable laminated structure, suppresses cation and resets; Ni helps to improve the embedding lithium capacity of material; Mn can reduce cost significantly, and can effectively improve the security performance of material.The excellent combination property of material, the lithium ion battery of being assembled have characteristics such as capacity height, operating voltage height and thermal stability excellence.
The manganese salt, the cobalt salt that are used for preparing ternary material generally are+divalent, be lower than in the product+4 ,+3 chemical valence, therefore, during preparation nickel-cobalt-manganese ternary positive electrode, generally need carry out low-temperature bake at 350～450 ℃, decompose with the raw material that will contain manganese (II) and cobalt (II), and manganese, cobalt ions are oxidized to higher valence state.Patent " a kind of preparation method of spherical nickel-cobalt lithium manganate material " (patent No. ZL200710034318.1, notification number CN101229928, day for announcing 2008.07.30), the method for preparing ternary material nickel cobalt manganese lithium with carbonate coprecipitation is disclosed, the sintering procedures that comprised for two steps in its sintering procedure, promptly 350～450 ℃ of low-firing processes of nickel cobalt manganese carbonate coprecipitation and sneak into the lithium source after 950 ℃ of left and right sides high-temperature firing processes once more.
Directly with high price manganese salt (as Mn 3O 4Or MnO 2), cobalt salt is raw material, adopts solid phase method to prepare the nickel-cobalt-manganese ternary positive electrode, though guaranteed manganese, the higher oxidation state of cobalt ions, stock yard is difficult for carrying out evenly mixing sample, has influenced batch stability and the performance homogeneity of product.
Summary of the invention
The object of the present invention is to provide that preparation time is short, the preparation method of the simple a kind of tertiary cathode material of technology.
For achieving the above object, the technical scheme taked of the present invention is:
A kind of preparation method of tertiary cathode material, this method may further comprise the steps:
A. lithium salts, nickel salt, manganese salt and cobalt salt are dissolved in the alcohol compound solvent according to mol ratio 1:1/3:1/3:1/3, make that lithium concentration is 0.1～1.0 mol/L in the mixed liquor;
B. fully stir, continue bubbling air or oxygen, concentrated ammonia liquor or ammonia are joined in the described mixed liquor, contained ammonia mole is 3:1～30:1 with the ratio of lithium salts mole in described ammoniacal liquor or the ammonia, obtains containing the dark solution of high price manganese and high price cobalt;
C. continue bubbling air, described dark solution is warming up to 80～120 ℃, until obtaining gelatinous atrament;
D. described atrament is placed in the high temperature furnace, in 800～950 ℃ of roasting 6～24 h, promptly obtains tertiary cathode material LiNi 1/3Mn 1/3Co 1/3O 2Submicron particles.
The mol ratio of lithium salts, nickel salt, manganese salt and cobalt salt is 1:0.4:0.4:0.2 in the described steps A, obtains tertiary cathode material LiNi through described step D 0.4Mn 0.4Co 0.2O 2Submicron particles.
The mol ratio of lithium salts, nickel salt, manganese salt and cobalt salt is 1:0.5:0.3:0.2 in the described steps A, obtains tertiary cathode material LiNi through described step D 0.5Mn 0.3Co 0.2O 2Submicron particles.
The mol ratio of lithium salts, nickel salt, manganese salt and cobalt salt is 1:0.7:0.15:0.15 in the described steps A, obtains tertiary cathode material LiNi through described step D 0.7Mn 0.15Co 0.15O 2Submicron particles.
Lithium salts in the described steps A is the lithium acetate of lithium nitrate, lithium acetate or the band crystallization water.
Manganese salt in the described steps A is the manganese acetate of the manganese acetate or the band crystallization water.
Nickel salt in the described steps A is the nickel acetate of nickel nitrate, nickel acetate or the band crystallization water of nickel nitrate, the band crystallization water.
Cobalt salt in the described steps A is the cobalt acetate of cobalt nitrate, cobalt acetate or the band crystallization water of cobalt nitrate, the band crystallization water.
Alcohol compound solvent in the described steps A is methyl alcohol, ethanol or both mixtures, and its mass percent concentration concentration is 80～99.9 %.
Adopt the preparation method of battery tertiary cathode material provided by the invention, have the following advantages:
Since the present invention in the preparation process of precursor, manganese ion and cobalt ions have been carried out pre-oxidation, improved the oxidation state of manganese ion and cobalt ions in the presoma, the existence of high oxidation state manganese element and cobalt element has been arranged in so final gained precursor, need under 350～450 ℃ of conditions, not carry out low-temperature oxidation, therefore can shorten the preparation time of product greatly.
2. the present invention adopts the Prepared by Sol Gel Method persursor material, strict guarantee manganese, cobalt, nickel, the stoichiometric proportion of lithium metal ion and the degree that mixes between them.
3. among the present invention, the homogeneous phase solution of high price manganese and high price cobalt is made through the air or oxygen oxidation by the compound of Mn (II) and Co (II), and preparation process is simple, quick, and does not introduce any assorted metal ion.From the high power Electronic Speculum figure of product as can be known: products obtained therefrom even particle size, grain diameter are uniformly dispersed at 200～300nm.
Description of drawings
Fig. 1 is the XRD spectra of the submicron order tertiary cathode material of the present invention's preparation.
Fig. 2 is the high power Electronic Speculum figure of the submicron order tertiary cathode material of the present invention's preparation.
Embodiment
Below by embodiment the present invention is described in further detail, following execution mode is descriptive, is not determinate, can not limit protection scope of the present invention with this.
Embodiment one:
A kind of preparation method of battery tertiary cathode material, this method may further comprise the steps:
1. get 0.03 mol lithium nitrate, 0.010 mol, six water nickel nitrates, 0.010 mol, four water manganese acetates, 0.010 mol, four water cobalt acetates, being dissolved in 75 mL mass percent concentrations is in the ethanolic solution of 99.9 %, obtain containing the homogeneous phase mixed liquor of lithium salts and manganese salt, wherein lithium concentration is 0.4 mol/L, and the color of mixed liquor is the redness of divalent manganesetion and cobalt ions at this moment.
2. fully stir above-mentioned mixed liquor, continue to blast air with air blast, adding mass percent concentration concentration is the concentrated ammonia liquor 13.5mL of 25 %, makes above-mentioned mixed liquor become aterrimus solution, and promptly divalent manganesetion and cobalt ions are oxidized to the color behind the higher valence state.With ammoniacal liquor density is that 0.91g/mL calculates, and this moment, the mole of ammoniacal liquor was 6 times of lithium salts mole.
3. above-mentioned aterrimus solution is heated to 90 ℃, and constant temperature, along with the continuous volatilization of solvent, finally obtain gelatinous black solid material.
4. above-mentioned black solid material is placed in the Muffle furnace, keeps 10h, can obtain the tertiary cathode material LiNi of spinel structure at 900 ℃ 1/3Mn 1/3Co 1/3O 2Submicron particles product, particle diameter are 200～300nm.
As shown in Figure 1, be LiNi 1/3Mn 1/3Co 1/3O 2The X-ray diffraction analysis figure of product is pure phase tertiary cathode material LiNi by the prepared as can be seen product of this XRD spectra 1/3Mn 1/3Co 1/3O 2
As shown in Figure 2, be LiNi 1/3Mn 1/3Co 1/3O 2The high power Electronic Speculum figure of product is the submicron order spinel structure by the prepared as can be seen product of this figure, and the product crystal formation is good, presents polyhedral structure.
Embodiment two:
A kind of preparation method of battery tertiary cathode material, this method may further comprise the steps:
1. get 0.03 mol lithium acetate, 0.012 mol nickel acetate, 0.012 mol manganese acetate, 0.006 mol cobalt acetate, being dissolved in 300 mL mass percent concentrations is in the ethanolic solution of 80 %, obtain containing the homogeneous phase mixed liquor of lithium salts and manganese salt, wherein lithium concentration is 0.1 mol/L, and the color of mixed liquor is the redness of divalent manganesetion and cobalt ions at this moment.
2. fully stir above-mentioned mixed liquor, continue to blast air with air blast, adding mass percent concentration concentration is the concentrated ammonia liquor 6.7mL of 25 %, makes above-mentioned mixed liquor become aterrimus solution, and promptly divalent manganesetion and cobalt ions are oxidized to the color behind the higher valence state.With ammoniacal liquor density is that 0.91g/mL calculates, and this moment, the mole of ammoniacal liquor was 3 times of lithium salts mole.
3. above-mentioned aterrimus solution is heated to 80 ℃, and constant temperature, along with the continuous volatilization of solvent, finally obtain gelatinous black solid material.
4. above-mentioned black solid material is placed in the Muffle furnace, keeps 6h, can obtain the tertiary cathode material LiNi of spinel structure at 950 ℃ 0.4Mn 0.4Co 0.2O 2The submicron particles product.
Embodiment three:
A kind of preparation method of battery tertiary cathode material, this method may further comprise the steps:
1. getting 0.3 mol, two water lithium acetates, 0.15 mol, six water nickel nitrates, 0.09 mol, four water manganese acetates, 0.06 mol cobalt nitrate hexahydrate, to be dissolved in 300 mL mass percent concentrations be in the methanol solution of 95 %, obtain containing the homogeneous phase mixed liquor of lithium salts and manganese salt, wherein lithium concentration is 1.0 mol/L, and the color of mixed liquor is the redness of divalent manganesetion and cobalt ions at this moment.
2. fully stir above-mentioned mixed liquor, continue to blast air with air blast, adding mass percent concentration concentration is the concentrated ammonia liquor 67mL of 25 %, makes above-mentioned mixed liquor become aterrimus solution, and promptly divalent manganesetion and cobalt ions are oxidized to the color behind the higher valence state.With ammoniacal liquor density is that 0.91g/mL calculates, and this moment, the mole of ammoniacal liquor was 30 times of lithium salts mole.
3. above-mentioned aterrimus solution is heated to 110 ℃, and constant temperature, along with the continuous volatilization of solvent, finally obtain gelatinous black solid material.
4. above-mentioned black solid material is placed in the Muffle furnace, keeps 18h, can obtain the tertiary cathode material LiNi of spinel structure at 850 ℃ 0.5Mn 0.3Co 0.2O 2The submicron particles product.
Embodiment four:
A kind of preparation method of battery tertiary cathode material, this method may further comprise the steps:
1. getting 0.03 mol lithium acetate, 0.021 mol, six water nickel acetates, 0.0045 mol manganese acetate, 0.0045 mol cobalt nitrate, to be dissolved in 200 mL mass percent concentrations be in the ethanolic solution of 90 %, obtain containing the homogeneous phase mixed liquor of lithium salts and manganese salt, wherein lithium concentration is 0.15 mol/L, and the color of mixed liquor is the redness of divalent manganesetion and cobalt ions at this moment.
2. fully stir above-mentioned mixed liquor, continue to blast air with air blast, adding mass percent concentration concentration is the concentrated ammonia liquor 22.3mL of 25 %, makes above-mentioned mixed liquor become aterrimus solution, and promptly divalent manganesetion and cobalt ions are oxidized to the color behind the higher valence state.With ammoniacal liquor density is that 0.91g/mL calculates, and this moment, the mole of ammoniacal liquor was 10 times of lithium salts mole.
3. above-mentioned aterrimus solution is heated to 120 ℃, and constant temperature, along with the continuous volatilization of solvent, finally obtain gelatinous black solid material.
4. above-mentioned black solid material is placed in the Muffle furnace, keeps 24h, can obtain the tertiary cathode material LiNi of spinel structure at 800 ℃ 0.7Mn 0.15Co 0.15O 2The submicron particles product.
Embodiment five:
A kind of preparation method of battery tertiary cathode material, this method may further comprise the steps:
1. get 0.03 mol lithium nitrate, 0.010 mol, four water manganese acetates, 0.010 mol, six water nickel nitrates, 0.010 mol, four water cobalt acetates, being dissolved in 100 mL mass percent concentration concentration is the methyl alcohol of 90 %: the volume ratio of ethanol is in the mixed solvent of 1:1, obtain containing the homogeneous phase mixed liquor of lithium salts and manganese salt, wherein lithium concentration is 0.3 mol/L, and the color of mixed liquor is the redness of divalent manganesetion and cobalt ions at this moment.
2. fully stir above-mentioned mixed liquor, continue to blast air, feed ammonia with air blast, it is that 0.3L/min(standard atmospheric pressure lower density is 0.771g/L that control feeds speed), continue 13min, make above-mentioned mixed liquor become aterrimus solution, promptly divalent manganesetion is oxidized to the color behind the higher valence state.The mole of the ammonia that feed this moment is 6 times of lithium salts mole.
3. above-mentioned dark solution is heated to 120 ℃, and constant temperature, along with the continuous volatilization of solvent, finally obtain gelatinous black solid material.
4. above-mentioned atrament is placed in the Muffle furnace, keeps 12h, can obtain the tertiary cathode material LiNi of spinel structure at 900 ℃ 1/3Mn 1/3Co 1/3O 2The submicron particles product.

Claims (9)

1. the preparation method of a tertiary cathode material is characterized in that, this method may further comprise the steps:
A. lithium salts, nickel salt, manganese salt and cobalt salt are dissolved in the alcohol compound solvent according to mol ratio 1:1/3:1/3:1/3, make that lithium concentration is 0.1～1.0 mol/L in the mixed liquor;
B. fully stir, continue bubbling air or oxygen, concentrated ammonia liquor or ammonia are joined in the described mixed liquor, contained ammonia mole is 3:1～30:1 with the ratio of lithium salts mole in described ammoniacal liquor or the ammonia, obtains containing the dark solution of high price manganese and high price cobalt;
C. continue bubbling air, described dark solution is warming up to 80～120 ℃, until obtaining gelatinous atrament;
D. described atrament is placed in the high temperature furnace, in 800～950 ℃ of roasting 6～24 h, promptly obtains tertiary cathode material LiNi 1/3Mn 1/3Co 1/3O 2Submicron particles.
2. according to the preparation method of the described a kind of tertiary cathode material of claim 1, it is characterized in that the mol ratio of lithium salts, nickel salt, manganese salt and cobalt salt is 1:0.4:0.4:0.2 in the described steps A, obtains tertiary cathode material LiNi through described step D 0.4Mn 0.4Co 0.2O 2Submicron particles.
3. according to the preparation method of the described a kind of tertiary cathode material of claim 1, it is characterized in that the mol ratio of lithium salts, nickel salt, manganese salt and cobalt salt is 1:0.5:0.3:0.2 in the described steps A, obtains tertiary cathode material LiNi through described step D 0.5Mn 0.3Co 0.2O 2Submicron particles.
4. according to the preparation method of the described a kind of tertiary cathode material of claim 1, it is characterized in that the mol ratio of lithium salts, nickel salt, manganese salt and cobalt salt is 1:0.7:0.15:0.15 in the described steps A, obtains tertiary cathode material LiNi through described step D 0.7Mn 0.15Co 0.15O 2Submicron particles.
5. according to the preparation method of the described a kind of tertiary cathode material of claim 1, it is characterized in that the lithium salts in the described steps A is the lithium acetate of lithium nitrate, lithium acetate or the band crystallization water.
6. according to the preparation method of the described a kind of tertiary cathode material of claim 1, it is characterized in that the manganese salt in the described steps A is the manganese acetate of the manganese acetate or the band crystallization water.
7. according to the preparation method of the described a kind of tertiary cathode material of claim 1, it is characterized in that the nickel salt in the described steps A is the nickel acetate of nickel nitrate, nickel acetate or the band crystallization water of nickel nitrate, the band crystallization water.
8. according to the preparation method of the described a kind of tertiary cathode material of claim 1, it is characterized in that the cobalt salt in the described steps A is the cobalt acetate of cobalt nitrate, cobalt acetate or the band crystallization water of cobalt nitrate, the band crystallization water.
9. according to the preparation method of the described a kind of tertiary cathode material of claim 1, it is characterized in that the alcohol compound solvent in the described steps A is methyl alcohol, ethanol or both mixtures, its mass percent concentration concentration is 80～99.9 %.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105489883A (en) * 2016-01-26 2016-04-13 四川大学 Preparing method for rapidly obtaining ternary anode material of lithium ion battery and anode material
CN107658451A (en) * 2017-09-18 2018-02-02 北京理工大学 A kind of 622NCM tertiary cathode materials and preparation method thereof
CN108736009A (en) * 2018-05-29 2018-11-02 中伟新材料有限公司 Cobalt nickel lithium manganate ternary material and preparation method thereof
CN109680333A (en) * 2019-01-04 2019-04-26 南通瑞翔新材料有限公司 A kind of wet preparation method of high Ni-monocrystal positive electrode
WO2023160016A1 (en) * 2022-02-25 2023-08-31 广东邦普循环科技有限公司 Method for preparing ternary precursor from microbubbles by pre-oxidation and application of ternary precursor

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Publication number Priority date Publication date Assignee Title
JP2011238416A (en) * 2010-05-07 2011-11-24 Sumitomo Metal Mining Co Ltd Positive electrode active material for nonaqueous electrolyte secondary battery and its manufacturing method, and nonaqueous electrolyte secondary battery using positive electrode active material
CN102386381A (en) * 2010-08-30 2012-03-21 机械科学研究总院先进制造技术研究中心 Preparation method of nano positive material for lithium ion battery
CN102856544A (en) * 2012-10-13 2013-01-02 兰州理工大学 Preparation method of nano nickel lithium manganate

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2011238416A (en) * 2010-05-07 2011-11-24 Sumitomo Metal Mining Co Ltd Positive electrode active material for nonaqueous electrolyte secondary battery and its manufacturing method, and nonaqueous electrolyte secondary battery using positive electrode active material
CN102386381A (en) * 2010-08-30 2012-03-21 机械科学研究总院先进制造技术研究中心 Preparation method of nano positive material for lithium ion battery
CN102856544A (en) * 2012-10-13 2013-01-02 兰州理工大学 Preparation method of nano nickel lithium manganate

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105489883A (en) * 2016-01-26 2016-04-13 四川大学 Preparing method for rapidly obtaining ternary anode material of lithium ion battery and anode material
CN107658451A (en) * 2017-09-18 2018-02-02 北京理工大学 A kind of 622NCM tertiary cathode materials and preparation method thereof
CN108736009A (en) * 2018-05-29 2018-11-02 中伟新材料有限公司 Cobalt nickel lithium manganate ternary material and preparation method thereof
CN109680333A (en) * 2019-01-04 2019-04-26 南通瑞翔新材料有限公司 A kind of wet preparation method of high Ni-monocrystal positive electrode
WO2023160016A1 (en) * 2022-02-25 2023-08-31 广东邦普循环科技有限公司 Method for preparing ternary precursor from microbubbles by pre-oxidation and application of ternary precursor

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